CN117230361B - Iron-based nanocrystalline strip and preparation method and application thereof - Google Patents
Iron-based nanocrystalline strip and preparation method and application thereof Download PDFInfo
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- CN117230361B CN117230361B CN202311216847.9A CN202311216847A CN117230361B CN 117230361 B CN117230361 B CN 117230361B CN 202311216847 A CN202311216847 A CN 202311216847A CN 117230361 B CN117230361 B CN 117230361B
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 231
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 87
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 230000005291 magnetic effect Effects 0.000 claims abstract description 62
- 238000000034 method Methods 0.000 claims abstract description 43
- 230000008569 process Effects 0.000 claims abstract description 28
- 239000000126 substance Substances 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 15
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 14
- 150000001340 alkali metals Chemical class 0.000 claims abstract description 14
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 14
- 150000002367 halogens Chemical class 0.000 claims abstract description 14
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 9
- 150000002910 rare earth metals Chemical class 0.000 claims abstract description 5
- 239000002243 precursor Substances 0.000 claims description 93
- 238000010438 heat treatment Methods 0.000 claims description 66
- 239000011162 core material Substances 0.000 claims description 31
- 238000003723 Smelting Methods 0.000 claims description 25
- 239000000460 chlorine Substances 0.000 claims description 23
- 239000003822 epoxy resin Substances 0.000 claims description 21
- 229920000647 polyepoxide Polymers 0.000 claims description 21
- 239000003795 chemical substances by application Substances 0.000 claims description 20
- 239000002994 raw material Substances 0.000 claims description 19
- 239000000155 melt Substances 0.000 claims description 16
- 229920000459 Nitrile rubber Polymers 0.000 claims description 12
- 239000012745 toughening agent Substances 0.000 claims description 11
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 10
- 229910052801 chlorine Inorganic materials 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 239000003973 paint Substances 0.000 claims description 8
- 229910052771 Terbium Inorganic materials 0.000 claims description 5
- 238000010791 quenching Methods 0.000 claims description 5
- 230000000171 quenching effect Effects 0.000 claims description 5
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 4
- 238000007598 dipping method Methods 0.000 claims description 4
- 239000002966 varnish Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 2
- 229910052700 potassium Inorganic materials 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000006698 induction Effects 0.000 abstract description 24
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 239000008204 material by function Substances 0.000 abstract description 2
- 239000010949 copper Substances 0.000 description 31
- 229910045601 alloy Inorganic materials 0.000 description 25
- 239000000956 alloy Substances 0.000 description 25
- 239000010936 titanium Substances 0.000 description 24
- 238000004804 winding Methods 0.000 description 24
- 230000000052 comparative effect Effects 0.000 description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 10
- 229910052802 copper Inorganic materials 0.000 description 10
- 239000011734 sodium Substances 0.000 description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- 230000006911 nucleation Effects 0.000 description 7
- 238000010899 nucleation Methods 0.000 description 7
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 6
- 230000009471 action Effects 0.000 description 6
- 239000013078 crystal Substances 0.000 description 6
- 238000011161 development Methods 0.000 description 6
- 229910052710 silicon Inorganic materials 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 229910000592 Ferroniobium Inorganic materials 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 5
- ZFGFKQDDQUAJQP-UHFFFAOYSA-N iron niobium Chemical compound [Fe].[Fe].[Nb] ZFGFKQDDQUAJQP-UHFFFAOYSA-N 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 description 4
- 229910001004 magnetic alloy Inorganic materials 0.000 description 4
- 239000002159 nanocrystal Substances 0.000 description 4
- FGDZQCVHDSGLHJ-UHFFFAOYSA-M rubidium chloride Chemical compound [Cl-].[Rb+] FGDZQCVHDSGLHJ-UHFFFAOYSA-M 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 229910052779 Neodymium Inorganic materials 0.000 description 3
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 238000007670 refining Methods 0.000 description 3
- GZCRRIHWUXGPOV-UHFFFAOYSA-N terbium atom Chemical compound [Tb] GZCRRIHWUXGPOV-UHFFFAOYSA-N 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052773 Promethium Inorganic materials 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- -1 ferroboron Chemical compound 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 230000005381 magnetic domain Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052750 molybdenum Inorganic materials 0.000 description 2
- 239000002707 nanocrystalline material Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000001103 potassium chloride Substances 0.000 description 2
- 235000011164 potassium chloride Nutrition 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- VQMWBBYLQSCNPO-UHFFFAOYSA-N promethium atom Chemical compound [Pm] VQMWBBYLQSCNPO-UHFFFAOYSA-N 0.000 description 2
- 229940102127 rubidium chloride Drugs 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 229910052720 vanadium Inorganic materials 0.000 description 2
- 229910000859 α-Fe Inorganic materials 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- 229910000976 Electrical steel Inorganic materials 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229910000808 amorphous metal alloy Inorganic materials 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000003009 desulfurizing effect Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000005294 ferromagnetic effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052758 niobium Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Landscapes
- Soft Magnetic Materials (AREA)
Abstract
The invention relates to the field of magnetic functional materials, in particular to an iron-based nanocrystalline strip, a preparation method and application thereof. The invention provides an iron-based nanocrystalline strip, wherein the chemical formula of the iron-based nanocrystalline strip material is Fe a Si b B c Nb d Cu e Ti f T g E h M i The method comprises the steps of carrying out a first treatment on the surface of the Wherein T is selected from at least one of alkali metals; e is at least one selected from halogen elements; m is selected from at least one of rare earth metals; a. b, c, d, e, f, g, h, i the atomic percentages of the corresponding elements are a+b+c+d+e+f+g+h+i=100deg.at%, 7at% or less a is 82at%,3at% or less b is 6at%,8at% or less c is 12at%,1at% or less d is 3at%,0.5at% or less e is 1.5at%,0.5at% or less f is 2.5at%,0.5at% or less g is 1.5at%,0.5at% or less h is 1.5at%,0.5at% or less i is 2.5at% or less, and g=h. By selecting the specifiable components and limiting the content of each component, the amorphous forming capability of the material can be improved, and the nanocrystalline strip with refined grains can be obtained in the follow-up crystallization process, so that the material can prepare a thinner and wider iron-based nanocrystalline strip, and the prepared iron-based nanocrystalline strip has high saturation magnetic induction intensity and low high frequency loss.
Description
Technical Field
The invention relates to the field of magnetic functional materials, in particular to an iron-based nanocrystalline strip, a preparation method and application thereof.
Background
Since the advent of the iron-based nanocrystalline magnetically soft alloy in the 80 s of the 20 th century, the excellent soft magnetic performance of the iron-based nanocrystalline magnetically soft alloy opens up a new chapter in the soft magnetic industry. Compared with the traditional soft magnetic materials such as silicon steel, ferrite and the like, the nanocrystalline soft magnetic alloy has high saturation induction intensity and magnetic conductivity and low loss, and meets the requirement of continuous development of miniaturization and high efficiency of power electronic devices. The existing Finemet nanocrystalline alloy at home and abroad is invented by Ri Li metal, and is widely applied due to the excellent soft magnetic property. Along with the development trend of high efficiency, energy saving and large capacity of power electronic components, wider and thinner requirements are put forward for nanocrystalline materials. The existing width (less than or equal to 100 mm) and thickness (more than or equal to 18 mu m) of the strip cannot meet the application requirements, the technical difficulty of annealing heat treatment and regulation of a large-size iron core magnetic field is high, the development and application of nanocrystalline materials on devices such as low-loss large-capacity high-frequency transformers are restricted, and the development of wide-width ultrathin nanocrystalline strips and large-size iron cores is urgent.
Chinese application CN103060691a discloses an iron-based nanocrystalline ribbon and a preparation method thereof, which is characterized in that the chemical molecular formula of the iron-based nanocrystalline ribbon is: fe (Fe) a Cu b Nb c Si d B e The nanocrystalline soft magnetic strip with excellent performance is prepared through the processes of raw material mixing, smelting and steel ingot making, single-roller extremely-cold thin strip making, heat treatment and the like, the method is based on FINEMET soft magnetic alloy components, the preparation process of the domestic iron-based nanocrystalline strip is shown in detail, the thickness of the prepared strip is 30-40 mu m, and the bandwidth is 3-10 mm. However, at the current development speed of power electronic devices, the nanocrystalline strip with such a specification cannot meet the more advanced requirements.
Chinese patent application CN112176249A discloses an iron-based nanocrystalline ribbon and a method for preparing the same, which is characterized in thatMi Jingbao has the chemical composition expression: fe (Fe) a Si b B c Cu d Nb e M f And M is at least one selected from Mo and V. The strip prepared by optimizing the content of the alloy components of the alloy has better amorphous forming capability and good thermal stability, and the addition of Mo element and V element effectively improves the defects of quick attenuation of high-frequency magnetic permeability and lower value of the soft magnetic alloy, and simultaneously improves the resistivity of the material, but the alloy has lower saturation magnetic induction.
Patent CN106086714a discloses an iron-based soft magnetic alloy having a width of more than 63.5mm, a thickness of between 13 and 20 micrometers, and a composition represented by the following expression: (Fe) 1-a M a ) 100-x-y-z-p-q-r Cu x Si y B z M' p M" q X r Wherein M is Co and/or Ni, M' is at least one element selected from the group consisting of Nb, W, ta, zr, hf, ti and Mo; m' is at least one element selected from the group consisting of V, cr, mn, al, a platinum group element, sc, Y, a rare earth element, au, zn, sn, and Re; and a, x, y, z, p, q and r satisfy 0.ltoreq.a.ltoreq.0.5, 0.1.ltoreq.x.ltoreq.3, 0.ltoreq.y.ltoreq.30, 1.ltoreq.z.ltoreq.25, 5.ltoreq.y+z.ltoreq.30, 0.1.ltoreq.p.ltoreq.30, q.ltoreq.10 and r.ltoreq.10, respectively, X is at least one element selected from the group consisting of C, ge, P, ga, sb, in, be and As, at least 50% of the alloy is crystallized, and the average particle size is 100nm or less. The alloy has better soft magnetic performance, but the patent does not analyze alloy components in detail and exemplifies the influence of different element contents on the soft magnetic performance of the alloy, and the alloy prepares an ultrathin ultra-wide strip through a better process method, but has lower saturation magnetic induction and does not realize high saturation magnetic induction intensity, high-frequency magnetic conductivity and low loss at the same time.
The saturation magnetic induction intensity and the high-frequency loss of the nanocrystalline alloy are in a mutually restricted relation, the loss is increased while the saturation magnetic induction intensity is improved, the loss is rapidly increased along with the frequency improvement under the high-frequency condition, and the development of the wide and ultrathin iron-based nanocrystalline strip with high saturation magnetic induction intensity and high frequency and low loss is of great significance for preparing iron cores with larger sizes, so that the fields of larger-capacity high-frequency transformers, larger-power wireless charging and the like are realized.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects that the iron-based nanocrystalline strip in the prior art is difficult to combine with high saturation magnetic induction intensity, high frequency and low loss and the strip has wide and ultrathin dimensions, so as to provide the iron-based nanocrystalline strip and the preparation method and application thereof.
The invention provides an iron-based nanocrystalline strip, wherein the chemical formula of the iron-based nanocrystalline strip material is Fe a Si b B c Nb d Cu e Ti f T g E h M i ；
Wherein T is selected from at least one of alkali metals; e is at least one selected from halogen elements; m is selected from at least one of rare earth metals;
a. b, c, d, e, f, g, h, i the atomic percentages of the corresponding elements are a+b+c+d+e+f+g+h+i=100deg.at%, 7at% or less a is 82at%,3at% or less b is 6 or less, 8at% or less c is 12at% or less, 1at% or less d is 3at% or less, 0.5at% or less e is 1.5at% or less, 0.5at% or less f is 2.5at% or less, 0.5at% or less g is 1.5at%,0.5at% or less h is 1.5at%,0.5at% or less i is 2.at% or less 5, and g=h.
Preferably, T is at least one selected from Li, na, K; and/or the number of the groups of groups,
the E is selected from Cl; and/or the number of the groups of groups,
and M is at least one selected from Tb, nd and Pm.
Preferably, the thickness of the strip is 12-16 mu m, the width of the strip is 150-250 mm, and the thickness deviation in the width direction of the strip is less than 0.001mm.
The invention provides a preparation method of the iron-based nanocrystalline strip, which comprises the following steps: weighing raw materials according to a stoichiometric ratio, mixing and smelting the raw materials, forming an amorphous precursor strip from a melt obtained by smelting, and performing magnetic field stress heat treatment on the formed amorphous precursor strip to obtain the iron-based nanocrystalline strip.
Optionally, the raw materials are selected from: industrial pure iron, pure silicon, ferroboron, ferroniobium, pure copper, pure titanium, sodium chloride, pure neodymium, lithium chloride, pure cerium, potassium chloride, pure terbium, pure promethium, and rubidium chloride.
Optionally, the smelting process is performed in a vacuum induction furnace under the action of electromagnetic force; the smelting temperature is 1300-1500 ℃.
Preferably, the amorphous precursor strip forming process is to form an amorphous precursor strip from a melt obtained by smelting by a single-roller rapid quenching method;
optionally, the amorphous precursor strip is formed by a single-roller rapid quenching method by using inert gas to pressurize and spray the melt obtained by smelting from a quartz nozzle onto a copper roller rotating at a high speed;
optionally, the inert gas comprises argon;
wherein in the single roll rapid quenching method, the cooling rate of the melt is 10 5 ～10 7 ℃/s；
The thickness of the formed amorphous precursor strip is 12-16 mu m, and the width of the strip is 150-250 mm.
Preferably, the amorphous precursor strip is subjected to magnetic field stress heat treatment by applying tension in the length direction of the amorphous precursor strip;
wherein the temperature of the magnetic field stress heat treatment is 520-580 ℃, the magnetic field strength of the magnetic field stress heat treatment is 30-70 mT, and the magnetic field direction is perpendicular to the longitudinal section of the amorphous precursor strip; the time of the magnetic field stress heat treatment is 10 s-10 min, and the tension is 1-100MPa.
The invention also provides a nanocrystalline iron core, which is obtained by winding an iron-based nanocrystalline strip to form a precursor core material, then impregnating the precursor core material with paint, and then solidifying in a chlorine atmosphere, wherein the iron-based nanocrystalline strip is the iron-based nanocrystalline strip or the iron-based nanocrystalline strip prepared by the preparation method;
wherein, the impregnant used in the impregnating varnish comprises epoxy resin and curing agent.
Optionally, the cross section of a winding needle used for winding and forming the iron-based nanocrystalline strip is rectangular, circular or triangular.
Optionally, the iron-based nanocrystalline strip is wound, the height of a window of a precursor core formed by using a winding needle with a rectangular cross section is 100-400mm, the width of the window is 100-300mm, the radius of a chamfer arc of the window is 10-100mm, and the winding thickness is 40-80mm;
optionally, the side length of a window of the precursor core formed by winding the iron-based nanocrystalline strip by using a winding needle with a triangular cross section is 100-400mm, the radius of a chamfer arc of the window is 10-100mm, and the winding thickness is 40-80mm.
Preferably, the time for impregnating the formed precursor core material with paint is 1-5 hours; and/or the number of the groups of groups,
the curing temperature is 60-180 ℃ and the curing time is 3-10h.
Preferably, the dip coating further comprises a toughening agent;
the mass ratio of the epoxy resin, the curing agent and the toughening agent in the impregnant is (8-12): (3-6): (0.8-1.2); and/or the number of the groups of groups,
the epoxy resin is selected from epoxy resin E-51; the curing agent is selected from polyetheramine D400; the toughening agent is selected from carboxyl terminated nitrile rubber.
The invention also provides application of the nanocrystalline iron core in high-frequency transformers or wireless charging.
The technical scheme of the invention has the following advantages:
1. the chemical formula of the material of the iron-based nanocrystalline strip provided by the invention is Fe a Si b B c Nb d Cu e Ti f T g E h M i The method comprises the steps of carrying out a first treatment on the surface of the Wherein T is selected from at least one of alkali metals; e is at least one selected from halogen elements; m is selected from at least one of rare earth metals; a+b+c+d+e+f+g+h+i=100, 76at% is equal to or less than 82at%,3at% is equal to or less than 6at% b, 8at% is equal to or less than 12at% c, 1at% is equal to or less than 3at% d, 0.5at% is equal to or less than 1.5at% e, 0.5at% is equal to or less than 2.5at% f, 0.5at% is equal to or less than 1.5at% g, 0.5at% is equal to or less than 1.5at% h, 0.5at% is equal to or less than 2.5at% i, g=h.
The iron-based nanocrystalline strip provided by the invention adopts specific components and limits the content of each component, wherein Fe element in the iron-based nanocrystalline strip is used as a ferromagnetic element to play a role in maintaining saturated magnetic induction intensity, and proper proportion of Si and B metal elements is key for obtaining an amorphous precursor; the large-size Nb element and Ti element can effectively prevent nanocrystalline grains from growing up, reduce the diffusion coefficient, and simultaneously the Ti element has the effects of resisting corrosion and oxidation, and reduces the reduction of saturation induction caused by oxidation of the material; the Cu element is used as a nucleation element, which is favorable for precipitation and refinement of nano-crystalline grains; the alkali metal element and the halogen element are added in a matching way, the alkali metal element can react with substances such as oxygen, nitrogen, sulfur and the like strongly in the smelting process and serve as a deoxidizer and a desulfurizing agent, so that the purity of the solution is improved, and meanwhile, the addition of the alkali metal element can reduce the atomic transition energy in the subsequent heat treatment process, promote heterogeneous nucleation of nano crystal grains, improve the nucleation proportion, thereby refining the crystal grains and reducing the loss; the halogen element is used for being added into the alloy together with alkali metal, the halogen element can improve the uniformity of the solution in the smelting process, and can promote the heterogeneous nucleation of nano crystal grains in the heat treatment process, thereby refining the crystal grains; the addition of the alkali metal element and the halogen element can reduce the thickness deviation in the width direction of the finally prepared iron-based nanocrystalline strip, the surface is smooth, a thinner and wider iron-based nanocrystalline strip can be prepared, the saturation induction intensity of the finally prepared iron core can be improved, the high-frequency loss of the iron core can be reduced, but the addition of excessive alkali metal element and halogen element can reduce the amorphous forming capability of the material in the preparation process, so that the performance of the finally prepared strip is reduced; the addition of rare earth elements can improve the amorphous forming capability and the thermal stability of the bulk amorphous alloy, so that the finally prepared thinner and wider iron-based nanocrystalline strip can be realized; in summary, by selecting the specifiable components and limiting the content of each component, the amorphous forming capability of the material can be improved, and the nanocrystalline band with refined crystal grains can be obtained in the follow-up crystallization process, so that the material can prepare a thinner and wider iron-based nanocrystalline band, and the prepared iron-based nanocrystalline band has high saturation magnetic induction intensity and low high frequency loss.
2. Furthermore, compared with other rare earth elements, the rare earth metal provided by the invention is easier to react with sulfur, oxygen and other impurity elements in the alloy to the surface of the solution in the smelting process, and meanwhile, a layer of compact oxide film can be formed on the surface of the alloy, so that the master alloy is purer, in addition, the amorphous forming capacity and the thermal stability of the alloy can be further improved by the Tb, the Nd and the Pm, the preparation of thinner and wider iron-based nanocrystalline strips is facilitated, and meanwhile, the rare earth element with larger size is used for facilitating the precipitation and refinement of alpha-Fe crystal grains, improving the saturation magnetic induction intensity of the finally obtained iron core and reducing the high-frequency loss of the iron core.
3. The preparation method of the iron-based nanocrystalline strip provided by the invention comprises the following steps: weighing raw materials according to a stoichiometric ratio, mixing and smelting the raw materials, forming an amorphous precursor strip from a melt obtained by smelting, and performing magnetic field stress heat treatment on the formed amorphous precursor strip to obtain the iron-based nanocrystalline strip.
According to Fe a Si b B c Nb d Cu e Ti f T g E h M i Preparing raw materials, mixing and smelting the raw materials, forming an amorphous precursor strip from a melt obtained by smelting, adopting magnetic field stress heat treatment in the process of crystallizing the formed amorphous precursor strip, firstly separating out uniform and fine nanocrystalline grains in the process of carrying out the magnetic field stress heat treatment, reducing coercive force and loss, generating great induced anisotropy in the width direction of the strip by applying proper stress, enabling the hysteresis loop of the alloy to be flat, improving the saturation magnetic induction intensity of the material, and simultaneously applying a transverse magnetic field, wherein compared with the process of carrying out the stress heat treatment and then the magnetic field heat treatment, the induced anisotropy can be further generated in the width direction, the moving domain wall enables the direction of the magnetic domain wall to be consistent with that of the magnetic field, the magnetic domain structure is improved, and the high-frequency loss of the strip is reduced; fe (Fe) a Si b B c Nb d Cu e Ti f T g E h M i Adding alkali metal element and halogen element, wherein the addition of alkali metal element can reduce atomic transition energy and promote the reaction in the subsequent heat treatment processThe heterogeneous nucleation of the nano crystal grains is carried out, the nucleation proportion is improved, so that the crystal grains are refined, and the loss is reduced; the halogen element is used for being added into the alloy together with alkali metal, the halogen element can improve the uniformity of the solution in the smelting process, and can promote the heterogeneous nucleation of nano crystal grains in the heat treatment process, thereby refining the crystal grains; the alkali metal element and the halogen element are added in a matching way, so that the thickness deviation in the width direction of the finally prepared iron-based nanocrystalline strip is reduced, the surface is smooth, a thinner and wider iron-based nanocrystalline strip can be prepared, the saturation induction intensity of the finally prepared iron core can be improved, and the high-frequency loss of the iron core can be reduced; the specific raw materials are mixed and smelted to form an amorphous precursor strip, and then the amorphous precursor strip is subjected to magnetic field stress heat treatment to obtain the thinner and wider iron-based nanocrystalline strip with high saturation magnetic induction intensity and high frequency and low loss.
4. The iron-based nanocrystalline strip prepared by the preparation method is wound to form a precursor core material, and then the precursor core material is subjected to paint dipping and then is solidified in a chlorine atmosphere to obtain the nanocrystalline core; wherein, the impregnant used in the impregnating varnish comprises epoxy resin, curing agent and toughening agent.
The iron-based nanocrystalline strip is wound to form a precursor core material, then the precursor core material is subjected to paint dipping in a specific impregnant, the precursor core material has better toughness due to the toughening agent in the impregnant, the iron-based nanocrystalline strip is not easy to break, and then solidification is carried out in a chlorine atmosphere, wherein chlorine can be matched with halogen elements in the iron-based nanocrystalline strip to further prevent iron core oxidation, chlorine can be fused into the impregnant on the one hand, the cohesiveness and solidification rate of the impregnant are improved, and therefore the final high-frequency loss to the nanocrystalline iron core is reduced.
5. Further, the mass ratio of the epoxy resin, the curing agent and the toughening agent in the impregnant provided by the invention is (8-12): (3-6): (0.8-1.2); the epoxy resin is selected from epoxy resin E-51; the curing agent is selected from polyetheramine D400; the toughening agent is selected from carboxyl terminated nitrile rubber. The mobility of the impregnant is better, the bonding strength is higher, the curing shrinkage rate is lower by selecting specific epoxy resin, curing agent and toughening agent and limiting the relative mass ratio, so that the finally obtained nanocrystalline iron core has better high-frequency wear performance.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings that are needed in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the present invention, and other drawings can be obtained according to the drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic view of the structure of a strip according to the present invention, wherein OX, OY, OZ are coordinate axes perpendicular to each other, OY is a longitudinal direction parallel to the strip, OZ is a thickness direction parallel to the strip, OX is a width direction parallel to the strip, and a longitudinal section of the strip is a section parallel to the OYZ plane.
Detailed Description
The following examples are provided for a better understanding of the present invention and are not limited to the preferred embodiments described herein, but are not intended to limit the scope of the invention, any product which is the same or similar to the present invention, whether in light of the present teachings or in combination with other prior art features, falls within the scope of the present invention.
The specific experimental procedures or conditions are not noted in the examples and may be followed by the operations or conditions of conventional experimental procedures described in the literature in this field. The reagents or apparatus used were conventional reagent products commercially available without the manufacturer's knowledge.
Example 1
The embodiment provides an iron-based nanocrystalline strip, which has a chemical formula:
Fe 80 Si 4 B 10 Nb 1 Cu 1 Ti 1 Na 1 Cl 1 Nd 1 . It will be appreciated that 80 is taken as an example and represents 80at% of Fe.
The embodiment provides a method for preparing a nanocrystalline iron core, which comprises the following steps:
1) Proportioning and mixing industrial pure iron, pure silicon, ferroboron alloy, ferroniobium alloy, pure copper, pure titanium, sodium chloride and pure neodymium according to the chemical formulas, and then placing the mixed raw materials into a vacuum induction furnace for smelting under the action of electromagnetic force (smelting temperature is 1350 ℃), so as to obtain a melt with uniform components; the melt was sprayed uniformly from a quartz nozzle onto a copper roller rotating at high speed using pressurized argon gas at 10 f 6 ～10 7 Cooling at a cooling rate of DEG C/s to form an amorphous precursor strip having a thickness of 14 [ mu ] m (a strip width direction thickness deviation of less than 0.001 mm) and a width of 200mm, the strip having a structure according to FIG. 1, wherein OY, OY and OZ are mutually perpendicular coordinate axes, OY being a length direction parallel to the strip, OZ being a thickness direction parallel to the strip, OX being a width direction parallel to the strip, and a longitudinal section of the strip being a section parallel to an OYZ plane;
2) Carrying out magnetic field stress heat treatment on the amorphous precursor strip obtained in the step 1) at 560 ℃ through a heat treatment furnace to obtain the iron-based nanocrystalline strip, wherein a strip inlet and a strip outlet are formed at two ends of the heat treatment furnace, the magnetic field stress heat treatment comprises the specific processes that the amorphous precursor strip is wound on an unreeling winder at the strip inlet, then the amorphous precursor strip on the unreeling winder is sent into the heat treatment furnace from the strip inlet and is reeled through a reeling winder at the strip outlet, the tension of the amorphous precursor strip along the length direction is controlled to be 60MPa by the unreeling winder and the reeling winder when the amorphous precursor strip passes through the heat treatment furnace, the advancing time of the amorphous precursor strip from the strip inlet to the strip outlet at the same position is 2min, and a transverse magnetic field which is perpendicular to the longitudinal section of the amorphous precursor strip and has the strength of 50mT is formed at the strip inlet to the strip outlet section in the heat treatment process;
3) Winding the iron-based nanocrystalline strip obtained in the step 2) into a precursor core material with a window height of 320mm, a window width of 180mm, a window chamfer arc radius of 60mm and a winding thickness of 60mm by using a winding machine with a winding needle with a rectangular cross section, and then impregnating the precursor core material with an impregnating agent for 2h, wherein the impregnating agent comprises epoxy resin E-51, polyetheramine D400 and carboxyl-terminated nitrile rubber, and the mass ratio of the epoxy resin E-51, polyetheramine D400 and carboxyl-terminated nitrile rubber is 10:5:1, a step of; and then, placing the paint-dipped precursor core material in an oven in a chlorine atmosphere, and curing for 6 hours at 90 ℃ to obtain the nanocrystalline iron core.
Example 2
The embodiment provides an iron-based nanocrystalline strip, which has a chemical formula:
Fe 81 Si 3 B 9 Nb 2 Cu 1 Ti 1 Li 1 Cl 1 Pm 1 。
the embodiment provides a preparation method of the iron-based nanocrystalline strip, which comprises the following steps:
1) Proportioning and mixing industrial pure iron, pure silicon, ferroboron alloy, ferroniobium alloy, pure copper, pure titanium, lithium chloride and pure promethium according to the chemical formula, and then placing the mixed raw materials into a vacuum induction furnace for smelting under the action of electromagnetic force (smelting temperature is 1350 ℃), so as to obtain a melt with uniform components; the melt was sprayed uniformly from a quartz nozzle onto a copper roller rotating at high speed using pressurized argon gas at 10 f 6 ～10 7 Cooling at a cooling rate of DEG C/s to form an amorphous precursor strip having a thickness of 15 [ mu ] m (a strip width direction thickness deviation of less than 0.001 mm) and a width of 200mm, the strip having a structure according to FIG. 1, wherein OY, OY and OZ are mutually perpendicular coordinate axes, OY being a length direction parallel to the strip, OZ being a thickness direction parallel to the strip, OX being a width direction parallel to the strip, and a longitudinal section of the strip being a section parallel to an OYZ plane;
2) Carrying out magnetic field stress heat treatment on the amorphous precursor strip obtained in the step 1) at 550 ℃ through a heat treatment furnace to obtain the iron-based nanocrystalline strip, wherein a strip inlet and a strip outlet are formed at two ends of the heat treatment furnace, the magnetic field stress heat treatment comprises the specific processes that the amorphous precursor strip is wound on an unreeling winder at the strip inlet, then the amorphous precursor strip on the unreeling winder is sent into the heat treatment furnace from the strip inlet and is reeled through a reeling winder at the strip outlet, the tension of the amorphous precursor strip along the length direction is controlled to be 70MPa by the unreeling winder and the reeling winder when the amorphous precursor strip passes through the heat treatment furnace, the advancing time of the amorphous precursor strip from the strip inlet to the strip outlet at the same position is 3min, and a transverse magnetic field which is perpendicular to the longitudinal section of the amorphous precursor strip and has the strength of 50mT is formed at the strip inlet to the strip outlet section in the heat treatment process;
3) Winding the iron-based nanocrystalline strip obtained in the step 2) into a precursor core material with a window height of 320mm, a window width of 180mm, a window chamfer arc radius of 60mm and a winding thickness of 60mm by using a winding machine with a winding needle with a rectangular cross section, and then impregnating the precursor core material with an impregnating agent for 2.5 hours, wherein the impregnating agent comprises epoxy resin E-51, polyetheramine D400 and carboxyl-terminated nitrile rubber, and the mass ratio of the epoxy resin E-51, polyetheramine D400 and the carboxyl-terminated nitrile rubber is 10:5:1, a step of; and then, placing the paint-dipped precursor core material in an oven in a chlorine atmosphere, and curing for 7 hours at 80 ℃ to obtain the nanocrystalline iron core.
Example 3
The embodiment provides an iron-based nanocrystalline strip, which has a chemical formula:
Fe 78 Si 4 B 11 Nb 2 Cu 1 Ti 1 K 1 Cl 1 Tb 1 。
the embodiment provides a method for preparing a nanocrystalline iron core, which comprises the following steps:
1) Proportioning and mixing industrial pure iron, pure silicon, ferroboron, ferroniobium, pure copper, pure titanium, potassium chloride and pure terbium purchased in the market according to the chemical formula, and then placing the mixed raw materials into a vacuum induction furnace for smelting under the action of electromagnetic force (the smelting temperature is 1350 ℃), so as to obtain a melt with uniform components; the melt was sprayed uniformly from a quartz nozzle onto a copper roller rotating at high speed using pressurized argon gas at 10 f 6 ～10 7 Cooling at a cooling rate of DEG C/s to form an amorphous precursor tape having a thickness of 13 μm (a thickness deviation in the tape width direction of less than 0.001 mm) and a width of 200mmThe material, the structure of the strip refers to fig. 1, OX, OY, OZ are mutually perpendicular coordinate axes, wherein OY is parallel to the length direction of the strip, OZ is parallel to the thickness direction of the strip, OX is parallel to the width direction of the strip, and the longitudinal section of the strip is parallel to the OYZ plane;
2) Carrying out magnetic field stress heat treatment on the amorphous precursor strip obtained in the step 1) at 570 ℃ through a heat treatment furnace to obtain the iron-based nanocrystalline strip, wherein a strip inlet and a strip outlet are formed at two ends of the heat treatment furnace, the magnetic field stress heat treatment comprises the specific processes that the amorphous precursor strip is wound on an unreeling winder at the strip inlet, then the amorphous precursor strip on the unreeling winder is sent into the heat treatment furnace from the strip inlet and is reeled through a reeling winder at the strip outlet, the tension of the amorphous precursor strip along the length direction is controlled to be 80MPa by the unreeling winder and the reeling winder when the amorphous precursor strip passes through the heat treatment furnace, the advancing time of the amorphous precursor strip from the strip inlet to the strip outlet at the same position is 4min, and a transverse magnetic field which is perpendicular to the longitudinal section of the amorphous precursor strip and has the strength of 50mT is formed at the strip inlet to the strip outlet section in the heat treatment process;
3) Winding the iron-based nanocrystalline strip obtained in the step 2) into a precursor core material with the window side length of 380mm, the window chamfer arc radius of 60mm and the winding thickness of 90mm by using a winding machine with a winding needle with a triangular cross section, and then impregnating the precursor core material in an impregnating agent for 2.5 hours, wherein the impregnating agent comprises epoxy resin E-51, polyetheramine D400 and carboxyl-terminated nitrile rubber, and the mass ratio of the epoxy resin E-51, polyetheramine D400 to the carboxyl-terminated nitrile rubber is 10:5:1, a step of; and then, placing the paint-dipped precursor core material in an oven in a chlorine atmosphere, and curing for 5 hours at 100 ℃ to obtain the nanocrystalline iron core.
Example 4
The embodiment provides an iron-based nanocrystalline strip, which has a chemical formula:
Fe 76 Si 5 B 11 Nb 1 Cu 1 Ti 2 Rb 1 Cl 1 Tb 2 。
the embodiment provides a method for preparing a nanocrystalline iron core, which comprises the following steps:
1) Proportioning and mixing industrial pure iron, pure silicon, ferroboron alloy, ferroniobium alloy, pure copper, pure titanium, rubidium chloride and pure terbium according to the chemical formulas, and then placing the mixed raw materials into a vacuum induction furnace for smelting under the action of electromagnetic force (smelting temperature is 1350 ℃), so as to obtain a melt with uniform components; the melt was sprayed uniformly from a quartz nozzle onto a copper roller rotating at high speed using pressurized argon gas at 10 f 6 ～10 7 Cooling at a cooling rate of DEG C/s to form an amorphous precursor strip having a thickness of 14 [ mu ] m (a strip width direction thickness deviation of less than 0.001 mm) and a width of 200mm, the strip having a structure according to FIG. 1, wherein OY, OY and OZ are mutually perpendicular coordinate axes, OY being a length direction parallel to the strip, OZ being a thickness direction parallel to the strip, OX being a width direction parallel to the strip, and a longitudinal section of the strip being a section parallel to an OYZ plane;
2) Carrying out magnetic field stress heat treatment on the amorphous precursor strip obtained in the step 1) at 570 ℃ through a heat treatment furnace to obtain the iron-based nanocrystalline strip, wherein a strip inlet and a strip outlet are formed at two ends of the heat treatment furnace, the magnetic field stress heat treatment comprises the specific processes that the amorphous precursor strip is wound on an unreeling winder at the strip inlet, then the amorphous precursor strip on the unreeling winder is sent into the heat treatment furnace from the strip inlet and is reeled through a reeling winder at the strip outlet, the tension of the amorphous precursor strip along the length direction is controlled to be 70MPa by the unreeling winder and the reeling winder when the amorphous precursor strip passes through the heat treatment furnace, the advancing time of the amorphous precursor strip from the strip inlet to the strip outlet at the same position is 2min, and a transverse magnetic field which is perpendicular to the longitudinal section of the amorphous precursor strip and has the strength of 50mT is formed at the strip inlet to the strip outlet section in the heat treatment process;
3) Winding the iron-based nanocrystalline strip obtained in the step 2) into a precursor core material with the window side length of 380mm, the window chamfer arc radius of 60mm and the winding thickness of 90mm by using a winding machine with a winding needle with a triangular cross section, and then impregnating the precursor core material in an impregnating agent for 3 hours, wherein the impregnating agent comprises epoxy resin E-51, polyetheramine D400 and carboxyl-terminated nitrile rubber, and the mass ratio of the epoxy resin E-51, polyetheramine D400 to the carboxyl-terminated nitrile rubber is 10:5:1, a step of; and then, placing the paint-dipped precursor core material in an oven in a chlorine atmosphere, and curing for 8 hours at 70 ℃ to obtain the nanocrystalline iron core.
Example 5
The embodiment provides an iron-based nanocrystalline strip, which has a chemical formula:
Fe 80 Si 4 B 10 Nb 1 Cu 1 Ti 1 Na 1 Cl 1 Nd 1 。
the preparation method of the nanocrystalline iron core is similar to that in example 1, except that step 2) is:
and (3) carrying out stress heat treatment on the amorphous precursor strip obtained in the step (1) at 560 ℃ through a heat treatment furnace to obtain the iron-based nanocrystalline strip, wherein a strip inlet and a strip outlet are arranged at two ends of the heat treatment furnace, the specific process of the stress heat treatment is that the amorphous precursor strip is wound on an unreeling winder, then the amorphous precursor strip on the unreeling winder is sent into the heat treatment furnace from the strip inlet and passes through the strip outlet and is wound through the reeling winder, the tension of the amorphous precursor strip along the length direction is controlled to be 60MPa when the amorphous precursor strip passes through the heat treatment furnace through the unreeling winder and the reeling winder, and the advancing time of the amorphous precursor strip from the strip inlet to the strip outlet at the same position on the amorphous precursor strip is controlled to be 2min.
Example 6
The embodiment provides an iron-based nanocrystalline strip, which has a chemical formula:
Fe 80 Si 4 B 10 Nb 1 Cu 1 Ti 1 Na 1 Cl 1 Nd 1 。
the preparation method of the nanocrystalline iron core is similar to that in example 1, except that the impregnating agent in step 3) does not contain carboxyl terminated nitrile rubber.
Example 7
The embodiment provides an iron-based nanocrystalline strip, which has a chemical formula:
Fe 80 Si 4 B 10 Nb 1 Cu 1 Ti 1 Na 1 Cl 1 Nd 1 。
the preparation method of the nanocrystalline iron core is similar to that in example 1, except that the precursor core after paint dipping in step 3) is placed in an oven in an air atmosphere and cured at 90 ℃ for 6 hours.
Example 8
The embodiment provides an iron-based nanocrystalline strip, which has a chemical formula:
Fe 80 Si 4 B 10 Nb 1 Cu 1 Ti 1 Na 1 Cl 1 Nd 1 。
the preparation method of the nanocrystalline iron core is similar to that in example 1, except that step 2) is:
2) And (2) carrying out heat treatment on the amorphous precursor strip obtained in the step (1) at 560 ℃ through a heat treatment furnace to obtain the iron-based nanocrystalline strip, wherein the heat treatment process is to place a coiled material into the heat treatment furnace for heat treatment for 2min after coiling the amorphous precursor strip.
Example 9
The embodiment provides an iron-based nanocrystalline strip, which has a chemical formula:
Fe 80 Si 4 B 10 Nb 1 Cu 1 Ti 1 Na 1 Cl 1 Nd 1 。
the preparation method of the nanocrystalline iron core is similar to that in example 1, except that step 2) is: and (2) carrying out magnetic field heat treatment on the amorphous precursor strip obtained in the step (1) at 560 ℃ through a heat treatment furnace to obtain the iron-based nanocrystalline strip, wherein the heat treatment process is to place a coiled material into the heat treatment furnace to be subjected to heat treatment for 2min under the action of a magnetic field after the amorphous precursor strip is coiled, and the magnetic field is a transverse magnetic field which is perpendicular to the longitudinal section of the amorphous precursor strip and has the intensity of 50 mT.
Comparative example 1
The comparative example provides an iron-based nanocrystalline strip having the formula:
Fe 80 Si 4 B 10 Nb 1 Cu 1 Ti 1 Na 1 Cl 1 ；
the preparation method of the nanocrystalline iron core is similar to that in example 1, except that pure neodymium is not included in the raw material in step 1).
Comparative example 2
The comparative example provides an iron-based nanocrystalline strip having the formula:
Fe 80 Si 4 B 10 Nb 1 Cu 1 Ti 1 Nd 1 。
the preparation method of the nanocrystalline iron core is similar to that in example 1, except that sodium chloride is not included in the raw material of step 1).
Comparative example 3
The comparative example provides an iron-based nanocrystalline strip having the formula:
Fe 80 Si 4 B 10 Nb 1 Cu 1 Na 1 Cl 1 Nd 1 。
the preparation method of the nanocrystalline iron core is similar to that in example 1, except that the raw material in step 1) does not include pure titanium.
Comparative example 4
The embodiment provides an iron-based nanocrystalline strip, which has a chemical formula:
Fe 80 Si 4 B 10 Nb 1 Cu 1 Ti 1 Na 1 Nd 1 。
the preparation method of the nanocrystalline iron core is similar to that in example 1, except that sodium chloride in the raw material of step 1) of example 1 is replaced with Na.
Test case
The nanocrystalline cores obtained in examples 1 to 9 and comparative examples 1 to 4 were tested, the saturation induction intensity of the nanocrystalline core was measured using a Vibrating Sample Magnetometer (VSM), the loss of the nanocrystalline core was measured using an ac B-H meter, and the test conditions were: 10kHz, 0.5T, 25 ℃;20kHz, 0.2T, 25 ℃; the results of the saturation induction and loss tests are shown in table 1.
TABLE 1
| Bs/T | P/W·kg -1 (10kHz、0.5T) | P/W·kg -1 (20kHz、0.2T) | |
| Example 1 | 1.54 | 4.3 | 2.08 |
| Example 2 | 1.56 | 4.5 | 2.16 |
| Example 3 | 1.49 | 4.1 | 2.01 |
| Example 4 | 1.45 | 3.9 | 1.92 |
| Example 5 | 1.53 | 5.4 | 3.12 |
| Example 6 | 1.54 | 4.7 | 2.41 |
| Example 7 | 1.53 | 5.0 | 3.17 |
| Example 8 | 1.44 | 7.5 | 6.11 |
| Example 9 | 1.52 | 4.8 | 2.52 |
| Comparative example 1 | 1.40 | 6.7 | 4.41 |
| Comparative example 2 | 1.39 | 7.2 | 5.12 |
| Comparative example 3 | 1.41 | 7.1 | 4.95 |
| Comparative example 4 | 1.33 | 8.2 | 5.77 |
It is apparent that the above examples are given by way of illustration only and are not limiting of the embodiments. Other variations or modifications of the above teachings will be apparent to those of ordinary skill in the art. It is not necessary here nor is it exhaustive of all embodiments. While still being apparent from variations or modifications that may be made by those skilled in the art are within the scope of the invention.
Claims (10)
1. An iron-based nanocrystalline strip, characterized in that the chemical formula of the iron-based nanocrystalline strip material is Fe a Si b B c Nb d Cu e Ti f T g E h M i ；
Wherein T is selected from at least one of alkali metals; e is at least one selected from halogen elements; m is selected from at least one of rare earth metals;
a. b, c, d, e, f, g, h, i the atomic percentages of the corresponding elements are a+b+c+d+e+f+g+h+i=100deg.at%, 7at% or less a is 82at%,3at% or less b is 6 or less, 8at% or less c is 12at% or less, 1at% or less d is 3at% or less, 0.5at% or less e is 1.5at% or less, 0.5at% or less f is 2.5at% or less, 0.5at% or less g is 1.5at%,0.5at% or less h is 1.5at%,0.5at% or less i is 2.at% or less 5, and g=h.
2. The iron-based nanocrystalline strip according to claim 1, wherein T is selected from at least one of Li, na, K, rb; and/or the number of the groups of groups,
the E is selected from Cl; and/or the number of the groups of groups,
and M is at least one selected from Tb, nd and Pm.
3. The iron-based nanocrystalline strip according to claim 1 or 2, wherein the strip thickness is 12-16 μm, the strip width is 150-250 mm, and the strip width direction thickness deviation is less than 0.001mm.
4. A method for producing the iron-based nanocrystalline strip according to any one of claims 1 to 3, comprising the steps of: weighing raw materials according to a stoichiometric ratio, mixing and smelting the raw materials, forming an amorphous precursor strip from a melt obtained by smelting, and performing magnetic field stress heat treatment on the formed amorphous precursor strip to obtain the iron-based nanocrystalline strip.
5. The method according to claim 4, wherein the process of forming the amorphous precursor strip is to form the amorphous precursor strip from the melted product by a single-roll rapid quenching method;
wherein in the single roll rapid quenching method, the cooling rate of the melt is 10 5 ～10 7 ℃/s；
The thickness of the formed amorphous precursor strip is 12-16 mu m, and the width of the strip is 150-250 mm.
6. The method of claim 4 or 5, wherein the magnetic field stress heat treatment of the amorphous precursor strip is performed by applying tension in the length direction of the amorphous precursor strip;
the temperature of the magnetic field stress heat treatment is 520-580 ℃, the magnetic field strength of the magnetic field stress heat treatment is 30-70 mT, the magnetic field direction is perpendicular to the longitudinal section of the amorphous precursor strip, the time of the magnetic field stress heat treatment is 10 s-10 min, and the tension is 1-100MPa.
7. A nanocrystalline iron core, characterized in that an iron-based nanocrystalline strip is wound to form a precursor core material, then the precursor core material is dipped in paint and then solidified in a chlorine atmosphere to obtain the nanocrystalline iron core, wherein the iron-based nanocrystalline strip is the iron-based nanocrystalline strip according to any one of claims 1 to 3 or the iron-based nanocrystalline strip prepared by the preparation method according to any one of claims 4 to 6;
wherein, the impregnant used in the impregnating varnish comprises epoxy resin and curing agent.
8. The nanocrystalline iron core according to claim 7, wherein the paint dipping time is 1-5 hours; and/or the number of the groups of groups,
the curing temperature is 60-180 ℃ and the curing time is 3-10h.
9. The nanocrystalline core as claimed in claim 7, wherein,
the paint also comprises a toughening agent;
the mass ratio of the epoxy resin, the curing agent and the toughening agent in the impregnant is (8-12): (3-6): (0.8-1.2); and/or the number of the groups of groups,
the epoxy resin is selected from epoxy resin E-51; the curing agent is selected from polyetheramine D400; the toughening agent is selected from carboxyl terminated nitrile rubber.
10. Use of a nanocrystalline core according to any one of claims 7-9 in a high frequency transformer or wireless charging.
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| CN114496441A (en) * | 2022-01-14 | 2022-05-13 | 山西雷麦电子科技有限公司 | High-saturation-magnetic-induction-intensity iron-based alloy strip and preparation method thereof |
| CN116479321A (en) * | 2023-03-08 | 2023-07-25 | 国网智能电网研究院有限公司 | Nanocrystalline magnetically soft alloy strip and preparation method and application thereof |
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