CN114226732A - Preparation process of silica gel magnetic ring - Google Patents
Preparation process of silica gel magnetic ring Download PDFInfo
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- CN114226732A CN114226732A CN202111564205.9A CN202111564205A CN114226732A CN 114226732 A CN114226732 A CN 114226732A CN 202111564205 A CN202111564205 A CN 202111564205A CN 114226732 A CN114226732 A CN 114226732A
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 230000005291 magnetic effect Effects 0.000 title claims abstract description 78
- 229910002027 silica gel Inorganic materials 0.000 title claims abstract description 73
- 239000000741 silica gel Substances 0.000 title claims abstract description 73
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 72
- 238000003723 Smelting Methods 0.000 claims abstract description 43
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 37
- 239000000956 alloy Substances 0.000 claims abstract description 37
- 239000011248 coating agent Substances 0.000 claims abstract description 30
- 238000000576 coating method Methods 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 27
- 239000006247 magnetic powder Substances 0.000 claims abstract description 26
- 238000009689 gas atomisation Methods 0.000 claims abstract description 23
- 239000000725 suspension Substances 0.000 claims abstract description 19
- 229910052742 iron Inorganic materials 0.000 claims abstract description 18
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 18
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 18
- 229910052771 Terbium Inorganic materials 0.000 claims abstract description 17
- 229910052802 copper Inorganic materials 0.000 claims abstract description 17
- 229910052758 niobium Inorganic materials 0.000 claims abstract description 17
- 229910052698 phosphorus Inorganic materials 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 14
- 238000000137 annealing Methods 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000003825 pressing Methods 0.000 claims abstract description 9
- 238000005266 casting Methods 0.000 claims abstract description 4
- 238000000889 atomisation Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims description 18
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 13
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 239000000314 lubricant Substances 0.000 claims description 10
- 229920002379 silicone rubber Polymers 0.000 claims description 10
- 239000004945 silicone rubber Substances 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 10
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 9
- 238000012360 testing method Methods 0.000 claims description 9
- 238000002441 X-ray diffraction Methods 0.000 claims description 8
- 239000007822 coupling agent Substances 0.000 claims description 8
- 229910021485 fumed silica Inorganic materials 0.000 claims description 8
- 230000008569 process Effects 0.000 claims description 8
- 239000011347 resin Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 8
- 239000006185 dispersion Substances 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 6
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 6
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 6
- -1 ethylene bis-stearyl Chemical group 0.000 claims description 6
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 4
- 238000012216 screening Methods 0.000 claims description 4
- 238000005204 segregation Methods 0.000 claims description 4
- 238000007873 sieving Methods 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 229940008309 acetone / ethanol Drugs 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000000748 compression moulding Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000001746 injection moulding Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- 238000009792 diffusion process Methods 0.000 claims description 2
- 230000006698 induction Effects 0.000 abstract description 7
- 238000013461 design Methods 0.000 abstract description 4
- 238000007709 nanocrystallization Methods 0.000 abstract description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 229910001004 magnetic alloy Inorganic materials 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005294 ferromagnetic effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002159 nanocrystal Substances 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- 208000012868 Overgrowth Diseases 0.000 description 1
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 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
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052752 metalloid Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F5/10—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product of articles with cavities or holes, not otherwise provided for in the preceding subgroups
- B22F5/106—Tube or ring forms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/02—Compacting only
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/06—Making metallic powder or suspensions thereof using physical processes starting from liquid material
- B22F9/08—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying
- B22F9/082—Making metallic powder or suspensions thereof using physical processes starting from liquid material by casting, e.g. through sieves or in water, by atomising or spraying atomising using a fluid
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/24—After-treatment of workpieces or articles
- B22F2003/248—Thermal after-treatment
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Power Engineering (AREA)
- Powder Metallurgy (AREA)
Abstract
A preparation process of a silica gel magnetic ring comprises the following steps: (1) alloy ingot casting: taking high-purity raw materials of Fe, Si, Nb, FeB, Cu, Fe-P, Tb and La, putting the raw materials into a crucible, and smelting the raw materials through a non-consumable vacuum arc smelting furnace to obtain an alloy ingot; (2) atomizing to prepare powder: putting the alloy cast ingot into vacuum suspension smelting gas atomization powder making equipment for atomization powder making; (3) coating and pressing; (4) and (3) heat treatment: and putting the silica gel magnetic ring blank into a vacuum annealing furnace for annealing to obtain the silica gel magnetic ring. The preparation process of the silica gel magnetic ring has reasonable step design, the Fe-based nanocrystalline alloy with high amorphous forming capability and soft magnetic property is prepared by smelting high-purity raw materials of Fe, Si, Nb, FeB, Cu, Fe-P, Tb and La, amorphous magnetic powder is prepared by a gas atomization method, and the silica gel magnetic ring is prepared by silica gel coating, pressing and nanocrystallization annealing, so that the magnetic conductivity, the saturation magnetic induction intensity, the direct current bias property and the mechanical property are improved, and the application prospect is wide.
Description
Technical Field
The invention belongs to the technical field of silica gel magnetic ring preparation, and particularly relates to a preparation process of a silica gel magnetic ring.
Background
Electromagnetic waves radiated and leaked by electronic equipment can seriously interfere with the normal work of other electronic equipment, so that the equipment is disordered in function and wrong in transmission. Therefore, reducing electromagnetic interference of electronic devices has been a matter of concern.
The magnetic ring, a kind of annular magnetizer, is the common anti-interference component in the electronic circuit, have very good inhibition to the high-frequency noise, under the magnetic ring function, can make the normal useful signal pass through very well, can inhibit the passing through of the high-frequency interference signal very well, and the magnetic ring is with low costs, employ very extensively.
At present, most of materials used for a magnetic ring are magnetic powder cores, which are also called soft magnetic composite materials, and refer to a new type of soft magnetic materials formed by coating ferromagnetic powder with insulating media and performing compression molding through a specific process method. The magnetic powder is coated on the surface of the magnetic powder through the insulating medium, so that the magnetic powder is mutually insulated, the surface resistivity is increased, the eddy current loss of the magnetic powder core is greatly reduced finally, and the high-frequency characteristic is obviously enhanced. Therefore, it is necessary to develop a process for manufacturing a silica gel magnetic ring, in which silica gel, which is an organic insulating medium, is used as an insulating agent and a binder to directly bind magnetic powder, and the strength and high-frequency characteristics of the magnetic powder core are enhanced.
The Chinese patent application No. CN202110380591.X discloses a preparation process of a high-impedance magnetic ring, wherein the high-impedance magnetic ring is prepared from the following raw materials in parts by weight: the magnetic powder core comprises Fe2O 363-65 parts, NiO 8-10 parts, ZnO 21.5-23 parts, CuO 3-5 parts and Co2O30.5-1.0 parts, and is technically characterized in that a doping agent Co2O3 is added, so that the impedance characteristic of the material is improved, and the magnetic powder is not bonded by using organic insulating medium silica gel as an insulating agent and a bonding agent, so that the strength and the high-frequency characteristic of the magnetic powder core are enhanced.
Disclosure of Invention
The purpose of the invention is as follows: in order to overcome the defects, the invention aims to provide a preparation process of a silica gel magnetic ring, which has reasonable step design, adopts high-purity raw materials of Fe, Si, Nb, FeB, Cu, Fe-P, Tb and La to prepare an iron-based nanocrystalline alloy with high amorphous forming capability and soft magnetic property by smelting, adopts a gas atomization method to prepare amorphous magnetic powder, and prepares the silica gel magnetic ring through silica gel coating, pressing and nano crystallization annealing, thereby improving the magnetic conductivity and the saturation magnetic induction intensity, having lower loss, simple process, high flexibility and wide application prospect.
The purpose of the invention is realized by the following technical scheme:
a preparation process of a silica gel magnetic ring comprises the following steps:
the method comprises the following steps:
(1) alloy ingot casting: taking high-purity raw materials of Fe, Si, Nb, FeB, Cu, Fe-P, Tb and La, putting the raw materials into a crucible, and smelting the raw materials through a non-consumable vacuum arc smelting furnace to obtain an alloy ingot;
(2) atomizing to prepare powder: putting the alloy ingot into vacuum suspension smelting gas atomization powder making equipment for atomization powder making to obtain atomized powder, screening the atomized powder by a 120-mesh standard sieve, and confirming that the screened atomized powder is amorphous by XRD (X-ray diffraction) test to obtain magnetic powder;
(3) coating and pressing: dissolving silica gel in acetone, adding the magnetic powder, wherein the adding amount of the silica gel is 2-5 wt% of the mass of the magnetic powder, and uniformly mixing to obtain a mixture; placing the mixture in an ultrasonic instrument, continuously stirring until acetone is volatilized, and then sieving by a 50-mesh standard sieve to obtain coating powder; putting the coated powder into a vacuum drying oven, and drying at 60-70 deg.C for 0.5-1 h; adding a lubricant into the dried and dried coating powder, wherein the adding amount of the lubricant is 0.5-1 wt% of the mass of the coating powder, then loading the coating powder into a die, and performing pressure maintaining for 1-3min under the pressure of 1800 plus one year 2000MPa by using a universal compressor to perform compression molding to obtain a silica gel magnetic ring blank;
(4) and (3) heat treatment: and (3) putting the silica gel magnetic ring blank into a vacuum annealing furnace, preserving the heat for 1-2h at the temperature of 450-490 ℃ under the condition of the vacuum degree of 10-3, and cooling to the room temperature along with the furnace to obtain the silica gel magnetic ring.
The preparation process of the silica gel magnetic ring has reasonable step design, the Fe-based nanocrystalline alloy with high amorphous forming capability and soft magnetic performance is prepared by smelting high-purity raw materials of Fe, Si, Nb, FeB, Cu, Fe-P, Tb and La, amorphous magnetic powder is prepared by a gas atomization method, and the silica gel magnetic ring with high magnetic conductivity and saturated magnetic induction intensity is obtained by silica gel coating, pressing and nanocrystallization annealing.
In the above process for preparing a silica gel magnetic ring, the typical composition of the master alloy is (FeaSibBcPd) eNbfCugTbhLai, wherein a is 0.76 to 0.78at%, b is 0.08 to 0.10at%, c is 0.1 to 0.12at%, d is 0.04 to 0.05at%, e is 98.0 to 98.5 at%, f is 0.6 to 0.8at%, g is 0.6 to 0.7at%, h is 0.3 to 0.4at%, and i is 0.2 to 0.3 at%.
The master alloy disclosed by the invention is reasonable in formula design, Fe is used as a metal magnetic element and is a main source of the magnetic property of the iron-based amorphous soft magnetic alloy, the content is high, Si and B are used as metalloid elements, the amorphous forming capability can be improved, the thermal stability is enhanced, meanwhile, the P has favorable influence on the microstructure and the soft magnetic property of the iron-based amorphous alloy for controlling the microstructure, and particularly the effectiveness on grain refinement is realized; the addition of a trace amount of Nb can obviously improve the amorphous forming capability and soft magnetic property of the alloy, and Nb has the behaviors of repulsion, segregation and the like, so that a nucleation site is provided for the precipitation of the nanocrystalline, thereby hindering the overgrowth of the alpha-Fe (Si) nanocrystalline grains, simultaneously increasing the crystallization temperature, improving the thermal stability and stabilizing the amorphous phase; cu is difficult to dissolve in the iron-based alloy, and a small amount of Cu is added to provide nucleation sites for the precipitation of the nano-crystals in the heat treatment process and effectively prevent the excessive growth of the crystal grains, so that the nano-crystal particles are proper in size and have good soft magnetic characteristics and mechanical properties; tb and La are used as rare earth elements, so that the ferromagnetic coupling exchange effect between ordered phases of the nanocrystalline soft magnetic alloy can be increased, and the high magnetic induction intensity and the high frequency and high magnetic conductivity of the nanocrystalline soft magnetic alloy are improved.
Further, in the preparation process of the silica gel magnetic ring, the smelting in the step (1) includes the following steps:
(1) placing high-purity raw materials of Fe, Si, Nb, FeB, Cu, Fe-P, Tb and La in an acetone/ethanol solution, removing oil stains and other organic matters on the surface by ultrasonic cleaning, and then drying;
(2) before smelting, strictly checking the cleanness of a cavity of a non-consumable vacuum arc smelting furnace, cleaning the furnace cavity, and then putting high-purity raw materials of Fe, Si, Nb, FeB, Cu, Fe-P, Tb and La into a crucible, wherein the low-melting-point volatile raw material is firstly put into the crucible; closing the furnace door, sequentially vacuumizing by using a mechanical pump and a diffusion pump to ensure that the oxygen partial pressure reaches below 5x10-2 Pa, filling high-purity argon to perform gas washing in the non-consumable vacuum arc melting furnace, continuously vacuumizing, and repeating the process for 2-3 times;
(3) and sequentially smelting the FFe, Si, Nb, FeB, Cu, Fe-P, Tb and La raw materials placed in the crucible into alloy ingots, and repeatedly smelting each alloy ingot for 4-6 times to reduce component segregation to obtain alloy ingots.
Further, in the preparation process of the silica gel magnetic ring, in the step (2), before the alloy ingot is placed into the vacuum suspension smelting gas atomization powder making equipment, a furnace body of the vacuum suspension smelting gas atomization powder making equipment is cleaned, so that the interference of foreign powder is avoided; and putting the alloy ingot into vacuum suspension smelting gas atomization powder making equipment, vacuumizing the vacuum suspension smelting gas atomization powder making equipment to below 10Pa, and then heating and atomizing.
Further, in the above preparation process of the silica gel magnetic ring, the lubricant in the step (3) is a mixture of zinc stearate and ethylene bis-stearyl, the addition amount of the zinc stearate is 0.2-0.5wt.% of the mass of the coated powder, and the addition amount of the ethylene bis-stearyl is 0.3-0.5wt.% of the mass of the coated powder.
Further, in the preparation process of the silica gel magnetic ring, the preparation of the silica gel comprises the following steps:
(1) adding MQ resin dissolved by n-hexane, fumed silica and a coupling agent KH570 into methyl block room temperature vulcanized silicone rubber, stirring and mixing for 0.5-1h on a high-speed dispersion machine, uniformly mixing, putting into a vacuum drying oven, drying at 25-30 ℃ to remove the n-hexane, and vacuumizing for 15-30min to obtain a mixture;
(2) adding ethyl orthosilicate and dibutyltin dilaurate into the mixture, stirring and mixing for 20-30min on a high-speed dispersion machine, vacuumizing and defoaming, carrying out injection molding, curing, opening the mold, and taking out to obtain the silica gel.
According to the invention, the methyl block room temperature vulcanized silicone rubber is reinforced and modified by the MQ resin, the fumed silica and the coupling agent KH570, so that the silicone rubber has excellent thermal stability, weather resistance, electrical insulation property and chemical reagent resistance, and also has better adhesive property and mechanical property.
Further, in the preparation process of the silica gel magnetic ring, the silica gel comprises the following components in parts by mass: 50-60 parts of methyl block room temperature vulcanized silicone rubber, 3-5 parts of MQ resin, 3-5 parts of fumed silica, 0.5-1 part of coupling agent KH5700.5, 0.5-1 part of ethyl orthosilicate and 0.2-0.4 part of dibutyltin dilaurate.
Compared with the prior art, the invention has the following beneficial effects: the preparation process of the silica gel magnetic ring has reasonable preparation steps, the Fe-based nanocrystalline alloy with high amorphous forming capability and soft magnetic property is prepared by smelting high-purity raw materials of Fe, Si, Nb, FeB, Cu, Fe-P, Tb and La, and the methyl block room temperature vulcanized silicone rubber is reinforced and modified by MQ resin, fumed silica and a coupling agent KH570, so that the silica gel has excellent thermal stability, weather resistance, electric insulation property and chemical reagent resistance, and has better adhesive property and mechanical property; the amorphous magnetic powder is prepared by a gas atomization method, and the silica gel magnetic ring with high magnetic conductivity and saturated magnetic induction intensity is obtained by the silica gel coating, pressing and nano crystallization annealing, so that the silica gel magnetic ring has lower loss, simple process, high flexibility and wide application prospect.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention are clearly and completely described in the embodiments with reference to specific experimental data, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The following examples 1 and 2 and comparative example 1 provide a preparation process of a silica gel magnetic ring.
Example 1
The preparation of the silica gel comprises the following steps:
(1) the silica gel comprises the following components in parts by mass: 60 parts of methyl block room temperature vulcanized silicone rubber, 3.5 parts of MQ resin, 4.0 parts of fumed silica, 5700.8 parts of coupling agent KH, 0.6 part of ethyl orthosilicate and 0.3 part of dibutyltin dilaurate;
(2) adding MQ resin dissolved by n-hexane, fumed silica and a coupling agent KH570 into methyl block room temperature vulcanized silicone rubber, stirring and mixing for 1h on a high-speed dispersion machine, uniformly mixing, putting into a vacuum drying oven, drying at 30 ℃ to remove the n-hexane, and vacuumizing for 20min to obtain a mixture;
(3) adding ethyl orthosilicate and dibutyltin dilaurate into the mixture, stirring and mixing for 30min on a high-speed dispersion machine, vacuumizing and defoaming, performing injection molding, curing, opening the mold, and taking out to obtain the silica gel.
Example 2
The preparation process of the silica gel magnetic ring comprises the following steps:
(1) alloy ingot casting: the typical composition of the master alloy is (Fe)0.76Si0.09B0.1P0.05)98.1Nb0.8Cu0.6Tb0.3La0.2(ii) a Weighing high-purity raw materials of Fe, Si, Nb, FeB, Cu, Fe-P, Tb and La according to the proportion, putting the high-purity raw materials of Fe, Si, Nb, FeB, Cu, Fe-P, Tb and La into an acetone/ethanol solution, removing surface oil stains and other organic matters through ultrasonic cleaning, and then drying; before smelting, strictly checking the cleanness of a cavity of a non-consumable vacuum arc smelting furnace, cleaning the furnace cavity, and then putting high-purity raw materials of Fe, Si, Nb, FeB, Cu, Fe-P, Tb and La into a crucible, wherein the low-melting-point volatile raw material is firstly put into the crucible; closing the furnace door in turn by using mechanical pump and expanderThe dispersion pump is vacuumized to ensure that the oxygen partial pressure reaches 5x10-2Introducing high-purity argon to perform gas washing in the non-consumable vacuum arc melting furnace below Pa, continuously vacuumizing, and repeating the process for 2-3 times; sequentially smelting FFe, Si, Nb, FeB, Cu, Fe-P, Tb and La raw materials placed in a crucible into alloy ingots, and repeatedly smelting each alloy ingot for 4-6 times to reduce component segregation to obtain alloy cast ingots
(2) Atomizing to prepare powder: before the alloy cast ingot is placed into vacuum suspension smelting gas atomization powder making equipment, a furnace body of the vacuum suspension smelting gas atomization powder making equipment is cleaned, and the interference of different powder is avoided; placing the alloy ingot into vacuum suspension smelting gas atomization powder making equipment, vacuumizing the vacuum suspension smelting gas atomization powder making equipment to below 10Pa, heating and atomizing to obtain atomized powder, screening the atomized powder by a 120-mesh standard sieve, and confirming that the screened atomized powder is amorphous through XRD (X-ray diffraction) test to obtain magnetic powder;
(3) coating and pressing: dissolving the silica gel obtained in the embodiment 1 in acetone, adding the magnetic powder, wherein the adding amount of the silica gel is 3 wt% of the mass of the magnetic powder, and uniformly mixing to obtain a mixture; placing the mixture in an ultrasonic instrument, continuously stirring until acetone is volatilized, and then sieving by a 50-mesh standard sieve to obtain coating powder; putting the coated powder into a vacuum drying oven, and drying at 65 ℃ for 1 h; adding a lubricant into the dried and dried coating powder, wherein the adding amount of the lubricant is 1wt.% of the mass of the coating powder, the adding amount of the zinc stearate is 0.5wt.% of the mass of the coating powder, and the adding amount of the ethylene bis-stearyl is 0.5wt.% of the mass of the coating powder, then loading the coating powder into a die, and carrying out pressure maintaining for 1min and press forming by using a universal compressor under the pressure of 2000MPa to obtain a silica gel magnetic ring blank;
(4) and (3) heat treatment: putting the silica gel magnetic ring blank into a vacuum annealing furnace, and keeping the vacuum degree at 10-3And (3) keeping the temperature at 487 ℃ for 1h, and cooling to room temperature along with the furnace to obtain the silica gel magnetic ring.
Comparative example 1
The preparation process of the silica gel magnetic ring comprises the following steps:
(1) atomizing to prepare powder: before the Finemet alloy (purchased from Shanghai Elliaai metal materials Co., Ltd.) is put into a vacuum suspension smelting gas atomization powder making device, cleaning a furnace body of the vacuum suspension smelting gas atomization powder making device to avoid the interference of different powders; putting the Finemet alloy into vacuum suspension smelting gas atomization powder making equipment, vacuumizing the vacuum suspension smelting gas atomization powder making equipment to below 10Pa, heating and atomizing to obtain atomized powder, screening the atomized powder by a 120-mesh standard sieve, and confirming that the screened atomized powder is amorphous through XRD (X-ray diffraction) test to obtain magnetic powder;
(2) coating and pressing: dissolving silica gel (methyl block room temperature vulcanized silicone rubber) in acetone, adding the magnetic powder, wherein the adding amount of the silica gel is 3 wt% of the mass of the magnetic powder, and uniformly mixing to obtain a mixture; placing the mixture in an ultrasonic instrument, continuously stirring until acetone is volatilized, and then sieving by a 50-mesh standard sieve to obtain coating powder; putting the coated powder into a vacuum drying oven, and drying at 65 ℃ for 1 h; adding a lubricant into the dried and dried coating powder, wherein the adding amount of the lubricant is 1wt.% of the mass of the coating powder, the adding amount of the zinc stearate is 0.5wt.% of the mass of the coating powder, and the adding amount of the ethylene bis-stearyl is 0.5wt.% of the mass of the coating powder, then loading the coating powder into a die, and carrying out pressure maintaining for 1min and press forming by using a universal compressor under the pressure of 2000MPa to obtain a silica gel magnetic ring blank;
(3) and (3) heat treatment: putting the silica gel magnetic ring blank into a vacuum annealing furnace, and keeping the vacuum degree at 10-3And (3) keeping the temperature at 487 ℃ for 1h, and cooling to room temperature along with the furnace to obtain the silica gel magnetic ring.
Effect verification:
the silica gel obtained from example 1 above was tested for properties:
preparing a test piece according to the regulation of GB/T11211-; the test results are: the silica gel of example 1 has a maximum adhesion strength of 2.9MPa, a tensile strength of 3.21MPa, and an elongation at break of 206%.
The performance of the silica gel magnetic ring obtained in the above example 2 and comparative example 1 was tested:
(1) saturation magnetic induction: measuring saturation magnetic induction intensity by using a 7410 type vibration magnetometer manufactured by Lake Shore corporation of America;
(2) coercive force: measuring the coercive force by adopting a BHS.40 model B.H instrument produced by the electronic technology of Japan research;
(3) magnetic permeability: testing the magnetic conductivity by adopting a 4294A type impedance analyzer produced by Agilent, USA, wherein the magnetic conductivity needs to be obtained by calculating the change of the measured inductance value through a corresponding formula;
(4) loss: testing with a broadband energy analyzer, calculating voltage with a formula, and measuring p under the corresponding voltagecvThe loss per unit volume is obtained by comparing the value with the effective volume of the corresponding sample.
The test data are shown in table 1.
The invention has many applications, and the above description is only a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention, and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that various modifications can be made without departing from the principles of the invention and these modifications are to be considered within the scope of the invention.
Claims (7)
1. A preparation process of a silica gel magnetic ring is characterized by comprising the following steps:
(1) alloy ingot casting: taking high-purity raw materials of Fe, Si, Nb, FeB, Cu, Fe-P, Tb and La, putting the raw materials into a crucible, and smelting the raw materials through a non-consumable vacuum arc smelting furnace to obtain an alloy ingot;
(2) atomizing to prepare powder: putting the alloy ingot into vacuum suspension smelting gas atomization powder making equipment for atomization powder making to obtain atomized powder, screening the atomized powder by a 120-mesh standard sieve, and confirming that the screened atomized powder is amorphous by XRD (X-ray diffraction) test to obtain magnetic powder;
(3) coating and pressing: dissolving silica gel in acetone, adding the magnetic powder, wherein the adding amount of the silica gel is 2-5 wt% of the mass of the magnetic powder, and uniformly mixing to obtain a mixture; placing the mixture in an ultrasonic instrument, continuously stirring until acetone is volatilized, and then sieving by a 50-mesh standard sieve to obtain coating powder; putting the coated powder into a vacuum drying oven, and drying at 60-70 deg.C for 0.5-1 h; adding a lubricant into the dried and dried coating powder, wherein the adding amount of the lubricant is 0.5-1 wt% of the mass of the coating powder, then loading the coating powder into a die, and performing pressure maintaining for 1-3min under the pressure of 1800 plus one year 2000MPa by using a universal compressor to perform compression molding to obtain a silica gel magnetic ring blank;
(4) and (3) heat treatment: putting the silica gel magnetic ring blank into a vacuum annealing furnace, and keeping the vacuum degree at 10-3Under the condition, the temperature is kept for 1-2h at the temperature of 450-490 ℃, and the silica gel magnetic ring is obtained after the temperature is cooled to the room temperature along with the furnace.
2. The process for preparing a silica gel magnetic ring as claimed in claim 1, wherein in the step (1), typical components of the master alloy are (FeaSibBcPd) eNbfCugTbhLai, wherein a =0.76-0.78at%, b =0.08-0.10at%, c =0.1-0.12at%, d =0.04-0.05at%, e =98.0-98.5 at%, f =0.6-0.8at%, g =0.6-0.7at%, h =0.3-0.4at%, and i =0.2-0.3 at%.
3. The preparation process of the silica gel magnetic ring as claimed in claim 1, wherein the smelting in the step (1) comprises the following steps:
(1) placing high-purity raw materials of Fe, Si, Nb, FeB, Cu, Fe-P, Tb and La in an acetone/ethanol solution, removing oil stains and other organic matters on the surface by ultrasonic cleaning, and then drying;
(2) before smelting, strictly checking the cleanness of a cavity of a non-consumable vacuum arc smelting furnace, cleaning the furnace cavity, and then putting high-purity raw materials of Fe, Si, Nb, FeB, Cu, Fe-P, Tb and La into a crucible, wherein the low-melting-point volatile raw material is firstly put into the crucible; tightly closing the furnace door, and sequentially vacuumizing by using a mechanical pump and a diffusion pump to ensure that the oxygen partial pressure reaches 5x10-2Introducing high-purity argon to perform gas washing in the non-consumable vacuum arc melting furnace below Pa, continuously vacuumizing, and repeating the process for 2-3 times;
(3) and sequentially smelting the FFe, Si, Nb, FeB, Cu, Fe-P, Tb and La raw materials placed in the crucible into alloy ingots, and repeatedly smelting each alloy ingot for 4-6 times to reduce component segregation to obtain alloy ingots.
4. The preparation process of the silica gel magnetic ring as claimed in claim 1, wherein in the step (2), before the alloy ingot is placed into the vacuum suspension smelting gas atomization powder making equipment, a furnace body of the vacuum suspension smelting gas atomization powder making equipment is cleaned to avoid interference of different powders; and putting the alloy ingot into vacuum suspension smelting gas atomization powder making equipment, vacuumizing the vacuum suspension smelting gas atomization powder making equipment to below 10Pa, and then heating and atomizing.
5. The preparation process of the silica gel magnetic ring as claimed in claim 1, wherein the lubricant in the step (3) is a mixture of zinc stearate and ethylene bis-stearyl, the addition amount of the zinc stearate is 0.2-0.5wt.% of the mass of the coated powder, and the addition amount of the ethylene bis-stearyl is 0.3-0.5wt.% of the mass of the coated powder.
6. The preparation process of the silica gel magnetic ring as claimed in claim 1, wherein the preparation of the silica gel comprises the following steps:
(1) adding MQ resin dissolved by n-hexane, fumed silica and a coupling agent KH570 into methyl block room temperature vulcanized silicone rubber, stirring and mixing for 0.5-1h on a high-speed dispersion machine, uniformly mixing, putting into a vacuum drying oven, drying at 25-30 ℃ to remove the n-hexane, and vacuumizing for 15-30min to obtain a mixture;
(2) adding ethyl orthosilicate and dibutyltin dilaurate into the mixture, stirring and mixing for 20-30min on a high-speed dispersion machine, vacuumizing and defoaming, carrying out injection molding, curing, opening the mold, and taking out to obtain the silica gel.
7. The preparation process of the silica gel magnetic ring as claimed in claim 6, wherein the silica gel comprises the following components in parts by mass: 50-60 parts of methyl block room temperature vulcanized silicone rubber, 3-5 parts of MQ resin, 3-5 parts of fumed silica, 0.5-1 part of coupling agent KH5700.5, 0.5-1 part of ethyl orthosilicate and 0.2-0.4 part of dibutyltin dilaurate.
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