CN117809925B - Nanocrystalline magnetic core material of high-frequency transformer and preparation method thereof - Google Patents
Nanocrystalline magnetic core material of high-frequency transformer and preparation method thereof Download PDFInfo
- Publication number
- CN117809925B CN117809925B CN202410234244.XA CN202410234244A CN117809925B CN 117809925 B CN117809925 B CN 117809925B CN 202410234244 A CN202410234244 A CN 202410234244A CN 117809925 B CN117809925 B CN 117809925B
- Authority
- CN
- China
- Prior art keywords
- nanocrystalline
- core material
- magnetic core
- quantum dots
- soft magnetic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000011162 core material Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 238000010438 heat treatment Methods 0.000 claims abstract description 66
- 239000006247 magnetic powder Substances 0.000 claims abstract description 42
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 36
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 claims abstract description 36
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002994 raw material Substances 0.000 claims abstract description 21
- 229960003638 dopamine Drugs 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 238000001816 cooling Methods 0.000 claims description 23
- 239000000243 solution Substances 0.000 claims description 22
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 20
- 239000012153 distilled water Substances 0.000 claims description 20
- 239000010949 copper Substances 0.000 claims description 18
- 239000002244 precipitate Substances 0.000 claims description 16
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 229910052802 copper Inorganic materials 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 239000000126 substance Substances 0.000 claims description 15
- 238000001291 vacuum drying Methods 0.000 claims description 15
- 238000005303 weighing Methods 0.000 claims description 15
- 239000002096 quantum dot Substances 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000003723 Smelting Methods 0.000 claims description 10
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 10
- 239000002131 composite material Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- 238000011049 filling Methods 0.000 claims description 10
- 239000007789 gas Substances 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 10
- 239000000047 product Substances 0.000 claims description 10
- 230000001681 protective effect Effects 0.000 claims description 10
- 239000006228 supernatant Substances 0.000 claims description 10
- 239000011787 zinc oxide Substances 0.000 claims description 8
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
- 239000012670 alkaline solution Substances 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 5
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 5
- 230000001105 regulatory effect Effects 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 150000003751 zinc Chemical class 0.000 claims description 4
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 4
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims description 3
- 239000004246 zinc acetate Substances 0.000 claims description 3
- 239000011592 zinc chloride Substances 0.000 claims description 3
- 235000005074 zinc chloride Nutrition 0.000 claims description 3
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims description 3
- 229960001763 zinc sulfate Drugs 0.000 claims description 3
- 229910000368 zinc sulfate Inorganic materials 0.000 claims description 3
- 230000001376 precipitating effect Effects 0.000 claims description 2
- 239000002707 nanocrystalline material Substances 0.000 abstract description 3
- 238000001953 recrystallisation Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 229910021389 graphene Inorganic materials 0.000 description 4
- 238000011056 performance test Methods 0.000 description 3
- 229910000859 α-Fe Inorganic materials 0.000 description 3
- 229910000976 Electrical steel Inorganic materials 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000006698 induction Effects 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000696 magnetic material Substances 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007712 rapid solidification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Landscapes
- Soft Magnetic Materials (AREA)
Abstract
The invention belongs to the technical field of nanocrystalline materials, and particularly provides a nanocrystalline magnetic core material of a high-frequency transformer and a preparation method thereof, wherein the nanocrystalline magnetic core material comprises the following synthetic raw materials in parts by weight: the nano-crystalline soft magnetic powder has a molecular formula of Fe aSibBcXdCue of 60-80 parts, wherein X is one or more of Nb, co, mo, ce, a is 60-68, b is 10-15, c is 2-6, d is 4-6, e is 6-13, a+b+c+d+e=100, graphene quantum dots are 10-20 parts, zinc oxide quantum dots are 10-15 parts, and dopamine is 4-6 parts. According to the invention, the nanocrystalline soft magnetic powder, the graphene quantum dots and the zinc oxide quantum dots are combined, dopamine is used for adjustment, and the nanocrystalline magnetic core material is synthesized by the multi-stage heating heat treatment for recrystallization, so that the electromagnetic performance of the whole magnetic core material is effectively improved, and the use requirement of the high-frequency transformer is met.
Description
Technical Field
The invention relates to the technical field of nanocrystalline materials, in particular to a nanocrystalline magnetic core material of a high-frequency transformer and a preparation method thereof.
Background
In the design and manufacture of high frequency transformers, the choice of core material has a decisive influence on the performance, efficiency and reliability of the device. Common magnetic core materials for conventional high frequency transformers include ferrite, silicon steel, and the like. These materials show certain limitations in long-term applications, such as ferrite losses at high frequencies, and silicon steel is not efficient in high frequency applications due to its large hysteresis and eddy current losses. As electronic devices move toward higher performance, higher frequencies, and smaller sizes, higher demands are placed on high frequency transformer core materials.
In recent years, with development of nano technology, nanocrystalline magnetic core materials have attracted attention in the industry and scientific research fields. Nanocrystalline materials have higher saturation induction, lower losses, and better frequency response characteristics than conventional core materials, which make them ideally well suited for use in high frequency transformers. However, the preparation process of the nanocrystalline magnetic core material is complicated, and it is necessary to ensure uniformity and performance stability of the material while maintaining its unique nanocrystalline structure. In addition, the high cost and process challenges limit the wide range of applications for these materials.
Disclosure of Invention
Aiming at the situation, in order to overcome the defects of the prior art, the invention provides the nanocrystalline magnetic core material of the high-frequency transformer and the preparation method thereof, nanocrystalline soft magnetic powder, graphene quantum dots and zinc oxide quantum dots are combined, dopamine is used for adjusting, multi-stage heating heat treatment is used for synthesizing the nanocrystalline magnetic core material, and the zero-dimensional quantum dot material and the nanocrystalline soft magnetic powder are uniformly combined for recrystallization, so that the overall electromagnetic performance of the material is improved.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: the invention provides a nanocrystalline magnetic core material of a high-frequency transformer, which comprises the following synthetic raw materials in parts by weight: the nano-crystalline soft magnetic powder has a molecular formula of Fe aSibBcXdCue of 60-80 parts, wherein X is one or more of Nb, co, mo, ce, a is 60-68, b is 10-15, c is 2-6, d is 4-6, e is 6-13, a+b+c+d+e=100, graphene quantum dots are 10-20 parts, zinc oxide quantum dots are 10-15 parts, and dopamine is 4-6 parts.
Preferably, the preparation method of the nanocrystalline soft magnetic powder comprises the following steps:
① . According to molecular formula of the nanocrystalline soft magnetic powder, weighing elementary substance raw materials of each element, adding the elementary substance raw materials into a vacuum smelting furnace, filling argon as protective gas until the air pressure is 300-500 mbar, and heating to 1400 ℃ to enable the elementary substance raw materials to be completely melted to obtain molten liquid;
② . Spraying the molten liquid prepared in the step ① onto a rotating cooling copper roller to obtain a nanocrystalline soft magnetic thin strip with a disordered structure, and mechanically crushing the nanocrystalline soft magnetic thin strip to obtain nanocrystalline soft magnetic powder.
Preferably, in the step ②, the distance between the nozzle and the cooled copper roll is 170-200 μm, and the rotational speed of the cooled copper roll is 20-40 m/s.
Preferably, the preparation method of the graphene quantum dot comprises the following steps:
I. 200mg graphite oxide powder is weighed and dissolved in 100 mL distilled water, and is stirred at 460-560 rpm for 30min, 0.5 mL of 20 wt% ammonia water is added, and stirring is continued for 10min, so that a mixture is obtained;
and II, transferring the mixture prepared in the step I into a high-pressure reaction kettle with a polytetrafluoroethylene lining, heating for 6-8 h at 200 ℃, cooling to room temperature, alternately washing and precipitating for three times by using ethanol and water, and placing in a vacuum drying oven to dry at 60 ℃ for 12 h to obtain the graphene quantum dots.
Preferentially, the preparation method of the zinc oxide quantum dot comprises the following steps:
⑴ . Weighing 20 mM zinc salt, dissolving in 100mL ethanol, stirring and dissolving to synthesize zinc ion solution;
⑵ . Weighing 0.1-0.2 g of KOH and dissolving the KOH in 10 mL ethanol, and ultrasonically dissolving to synthesize an alkali solution;
⑶ . Dropwise adding the alkaline solution prepared in the step ⑵ into the zinc ion solution prepared in the step ⑴, stirring at 480-580 rpm, centrifuging to remove supernatant, alternately washing precipitate with ethanol and water for three times, and drying at 60 ℃ in a vacuum drying oven for 12h to obtain the zinc oxide quantum dot.
Preferably, in the step ⑴, the zinc salt is any one of zinc chloride, zinc sulfate, zinc acetate, and zinc nitrate.
The invention also provides a preparation method of the nanocrystalline magnetic core material of the high-frequency transformer, which comprises the following steps:
S1, mixing nanocrystalline soft magnetic powder, graphene quantum dots, zinc oxide quantum dots and dopamine in distilled water according to the mass parts, wherein the mass ratio of the distilled water to the nanocrystalline soft magnetic powder is 30-40: stirring at 1,460-560 rpm for 2h, regulating the pH to 9 by using 1 mol/L NaOH solution, continuously stirring for 4-6 hours, filtering to remove supernatant, washing the precipitate by using distilled water for three times, and drying at 60 ℃ in a vacuum drying oven for 12h to obtain a composite material;
S2, placing the composite material prepared in the step S1 into a vacuum smelting furnace, filling argon as protective gas until the air pressure is 300-500 mbar, performing heat treatment in a gradual heating mode, heating to 300-350 ℃ for the first time, and preserving heat for 10-20 min; heating to 400-450 ℃ for the second time, and preserving heat for 10-20 min; heating to 500-550 ℃ for the third time, preserving heat for 30-40 min, stirring for 5 min every 10min, heating at a speed of 8 ℃/min, and cooling to room temperature at a speed of 10 ℃/min after heat treatment is finished to obtain a heat treatment product;
And S3, placing the heat treatment product prepared in the step S2 into liquid nitrogen for cold treatment for 1 h, and recovering to room temperature to obtain the nanocrystalline magnetic core material.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a nanocrystalline magnetic core material for a high-frequency transformer and a preparation method thereof, wherein the design concept is based on advanced nanotechnology, and the invention aims to overcome the limitation of the traditional ferrite in high-frequency application. The nanocrystalline magnetic core material is synthesized by nanocrystalline soft magnetic powder, graphene quantum dots, zinc oxide quantum dots and dopamine in a specific proportion through stage heating heat treatment, and the unique combination endows the material with excellent electromagnetic properties and thermal stability. The nanocrystalline magnetic core material of the invention remarkably improves the saturation induction intensity and the magnetic permeability through the nanoscale crystal structure thereof, and simultaneously reduces hysteresis loss. The structural advantage enables the material to maintain lower energy loss at high frequencies, thereby improving overall energy efficiency and performance. The graphene quantum dots and the zinc oxide quantum dots are introduced and uniformly combined with nanocrystalline soft magnetic powder, and are recrystallized by heat treatment, and the quantum confinement properties of the graphene quantum dots and the semiconductor quantum dots adjust the electronic structure of the magnetic material after heat treatment, so that the electromagnetic property of the material is further improved, and the electromagnetic loss of the material is weakened. The addition of dopamine optimizes the surface property of the material and is beneficial to improving the uniformity and granularity control in the preparation process. The nanocrystalline magnetic core material provided by the invention not only meets the severe requirements of modern high-frequency transformers on the magnetic core material in theory, but also shows the remarkable advantages of improving the efficiency, reducing the energy consumption and enhancing the reliability of equipment in practical application.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only of the invention and that other drawings can be obtained from them without inventive effort for a person skilled in the art.
FIG. 1 is a scanning electron microscope image of the nanocrystalline magnetic core material produced in example 1 of the present invention;
Fig. 2 is an XRD pattern of the nanocrystalline magnetic core material and nanocrystalline soft magnetic powder prepared in example 1 of the present invention.
Description of the reference numerals: a is a nanocrystalline magnetic core material, and b is nanocrystalline soft magnetic powder.
Detailed Description
The present invention will be further described in detail with reference to the following specific examples, but the present invention is not limited to the following examples, for the purpose of making the objects, technical solutions and advantages of the present invention more apparent.
Unless otherwise specified, the chemical reagents involved in the present invention are all commercially available.
Example 1: the embodiment provides a nanocrystalline magnetic core material of a high-frequency transformer, wherein the nanocrystalline magnetic core material comprises the following synthetic raw materials in parts by weight: 60 parts of nanocrystalline soft magnetic powder with a molecular formula of Fe 60Si15B6Nb6Cu13, 20 parts of graphene quantum dots, 10 parts of zinc oxide quantum dots and 6 parts of dopamine.
The preparation method of the nanocrystalline soft magnetic powder comprises the following steps:
① . According to the molecular formula of the nanocrystalline soft magnetic powder, weighing elementary substance raw materials of each element, adding the elementary substance raw materials into a vacuum smelting furnace, filling argon as protective gas until the air pressure is 300 mbar, and heating to 1400 ℃ to fully melt the elementary substance raw materials to obtain molten liquid;
② . Spraying the molten liquid prepared in the step ① onto a rotating cooling copper roller, wherein the distance between a nozzle and the cooling copper roller is 170 mu m, the rotating speed of the cooling copper roller is 20 m/s, so as to obtain a nanocrystalline soft magnetic ribbon with a disordered structure, and mechanically crushing the nanocrystalline soft magnetic ribbon to obtain nanocrystalline soft magnetic powder.
The preparation method of the graphene quantum dot comprises the following steps:
I. 200 mg graphite oxide powder is weighed and dissolved in 100 mL distilled water, 460 rpm is stirred for 30 min, 0.5 mL of 20 wt% ammonia water is added, and stirring is continued for 10min, so that a mixture is obtained;
and II, transferring the mixture prepared in the step I into a high-pressure reaction kettle with a polytetrafluoroethylene lining, heating at 200 ℃ to 6h, cooling to room temperature, alternately washing the precipitate with ethanol and water for three times, and placing the precipitate in a vacuum drying oven to dry at 60 ℃ for 12h to obtain the graphene quantum dots.
The preparation method of the zinc oxide quantum dot comprises the following steps:
⑴ . Weighing 20 mM zinc chloride, dissolving in 100 mL ethanol, and stirring to dissolve and synthesize zinc ion solution;
⑵ . Weighing 0.1 g KOH to be dissolved in 10mL ethanol, and ultrasonically dissolving to synthesize an alkali solution;
⑶ . Dropwise adding the alkaline solution prepared in the step ⑵ into the zinc ion solution prepared in the step ⑴, stirring 480 and rpm for 12 hours, centrifuging at 6000 rpm to remove supernatant, washing precipitate with ethanol and water alternately for three times, and drying at 60 ℃ in a vacuum drying oven for 12h to obtain the zinc oxide quantum dot.
The embodiment also provides a preparation method of the high-frequency transformer nanocrystalline magnetic core material, which comprises the following steps:
s1, mixing nanocrystalline soft magnetic powder, graphene quantum dots, zinc oxide quantum dots and dopamine in distilled water according to the mass parts, wherein the mass ratio of the distilled water to the nanocrystalline soft magnetic powder is 30: stirring at 1,460 rpm for 2h, regulating pH to 9 with 1 mol/L NaOH solution, stirring for 6 h, filtering to remove supernatant, washing precipitate with distilled water for three times, and drying at 60deg.C in vacuum drying oven for 12h to obtain composite material;
S2, placing the composite material prepared in the step S1 into a vacuum smelting furnace, filling argon as protective gas until the air pressure is 300 mbar, performing heat treatment in a gradual heating mode, heating to 300 ℃ for the first time, and preserving heat for 10 min; heating to 400 ℃ for the second time, and preserving heat for 10 min; heating to 500 ℃ for the third time, preserving heat for 30min, stirring for 5min every 10: 10min, heating at 8 ℃/min, and cooling to room temperature at the rate of 10 ℃/min after heat treatment to obtain a heat treatment product;
And S3, placing the heat treatment product prepared in the step S2 into liquid nitrogen for cold treatment for 1 h, and recovering to room temperature to obtain the nanocrystalline magnetic core material.
Example 2: the embodiment provides a nanocrystalline magnetic core material of a high-frequency transformer, wherein the nanocrystalline magnetic core material comprises the following synthetic raw materials in parts by weight: 80 parts of nanocrystalline soft magnetic powder with a molecular formula of Fe 68Si10B2Mo4Cu6, 10 parts of graphene quantum dots, 15 parts of zinc oxide quantum dots and 5 parts of dopamine.
The preparation method of the nanocrystalline soft magnetic powder comprises the following steps:
① . According to the molecular formula of the nanocrystalline soft magnetic powder, weighing elementary substance raw materials of each element, adding the elementary substance raw materials into a vacuum smelting furnace, filling argon as protective gas until the air pressure is 400 mbar, and heating to 1400 ℃ to fully melt the elementary substance raw materials to obtain molten liquid;
② . Spraying the molten liquid prepared in the step ① onto a rotating cooling copper roller, wherein the distance between a nozzle and the cooling copper roller is 200 mu m, the rotating speed of the cooling copper roller is 40 m/s, obtaining a nanocrystalline soft magnetic thin strip with a disordered structure, and mechanically crushing the nanocrystalline soft magnetic thin strip to obtain nanocrystalline soft magnetic powder.
The preparation method of the graphene quantum dot comprises the following steps:
I. 200 mg graphite oxide powder is weighed and dissolved in 100 mL distilled water, 560 and rpm are stirred for 30 and min, 0.5 mL of 20 wt% ammonia water is added, and stirring is continued for 10 and min, so that a mixture is obtained;
And II, transferring the mixture prepared in the step I into a high-pressure reaction kettle with a polytetrafluoroethylene lining, heating at 200 ℃ to 8 h, cooling to room temperature, alternately washing the precipitate with ethanol and water for three times, and placing the precipitate in a vacuum drying oven to dry at 60 ℃ for 12h to obtain the graphene quantum dots.
The preparation method of the zinc oxide quantum dot comprises the following steps:
⑴ . Weighing 20 mM zinc sulfate, dissolving in 100 mL ethanol, and stirring to dissolve and synthesize zinc ion solution;
⑵ . Weighing 0.2 g KOH to be dissolved in 10mL ethanol, and ultrasonically dissolving to synthesize an alkali solution;
⑶ . Dropwise adding the alkaline solution prepared in the step ⑵ into the zinc ion solution prepared in the step ⑴, stirring 580 rpm for 12h, centrifuging at 10000 rpm to remove supernatant, alternately washing precipitate with ethanol and water for three times, and drying at 60 ℃ in a vacuum drying oven for 12h to obtain zinc oxide quantum dots.
The embodiment also provides a preparation method of the high-frequency transformer nanocrystalline magnetic core material, which comprises the following steps:
S1, mixing nanocrystalline soft magnetic powder, graphene quantum dots, zinc oxide quantum dots and dopamine in distilled water according to the mass parts, wherein the mass ratio of the distilled water to the nanocrystalline soft magnetic powder is 40: stirring at 1,560 rpm for 2h, regulating pH to 9 with 1 mol/L NaOH solution, stirring continuously for 4h, filtering to remove supernatant, cleaning precipitate with distilled water for three times, and drying at 60deg.C in vacuum drying oven for 12h to obtain composite material;
S2, placing the composite material prepared in the step S1 into a vacuum smelting furnace, filling argon as protective gas until the air pressure is 500 mbar, performing heat treatment in a gradual heating mode, heating to 350 ℃ for the first time, and preserving heat for 20: 20 min; heating to 450 ℃ for the second time, and preserving heat for 20 min; heating to 550 ℃ for the third time, preserving heat 40 min, stirring 5min every 10: 10min, heating at 8 ℃/min, and cooling to room temperature at the rate of 10 ℃/min after heat treatment to obtain a heat treatment product;
And S3, placing the heat treatment product prepared in the step S2 into liquid nitrogen for cold treatment for 1 h, and recovering to room temperature to obtain the nanocrystalline magnetic core material.
Example 3: the embodiment provides a nanocrystalline magnetic core material of a high-frequency transformer, wherein the nanocrystalline magnetic core material comprises the following synthetic raw materials in parts by weight: 70 parts of nanocrystalline soft magnetic powder with a molecular formula of Fe 65Si13B5Ce5Cu12, 15 parts of graphene quantum dots, 12 parts of zinc oxide quantum dots and 4 parts of dopamine.
The preparation method of the nanocrystalline soft magnetic powder comprises the following steps:
① . According to the molecular formula of the nanocrystalline soft magnetic powder, weighing elementary substance raw materials of each element, adding the elementary substance raw materials into a vacuum smelting furnace, filling argon as protective gas until the air pressure is 500 mbar, and heating to 1400 ℃ to fully melt the elementary substance raw materials to obtain molten liquid;
② . Spraying the molten liquid prepared in the step ① onto a rotating cooling copper roller, wherein the distance between a nozzle and the cooling copper roller is 180 mu m, the rotating speed of the cooling copper roller is 30 m/s, so as to obtain a nanocrystalline soft magnetic ribbon with a disordered structure, and mechanically crushing the nanocrystalline soft magnetic ribbon to obtain nanocrystalline soft magnetic powder.
The preparation method of the graphene quantum dot comprises the following steps:
I. 200 mg graphite oxide powder is weighed and dissolved in 100 mL distilled water, 500 rpm is stirred for 30 min, 0.5 mL of 20 wt% ammonia water is added, and stirring is continued for 10min, so that a mixture is obtained;
And II, transferring the mixture prepared in the step I into a high-pressure reaction kettle with a polytetrafluoroethylene lining, heating to 7 h at 200 ℃, cooling to room temperature, alternately washing the precipitate with ethanol and water for three times, and placing the precipitate in a vacuum drying oven to dry 12h at 60 ℃ to obtain the graphene quantum dots.
The preparation method of the zinc oxide quantum dot comprises the following steps:
⑴ . Weighing 20 mM zinc acetate, dissolving in 100 mL ethanol, and stirring to dissolve and synthesize zinc ion solution;
⑵ . Weighing 0.15 g KOH and dissolving in 10mL ethanol, and ultrasonically dissolving to synthesize an alkali solution;
⑶ . Dropwise adding the alkaline solution prepared in the step ⑵ into the zinc ion solution prepared in the step ⑴, stirring for 12 h with 500 rpm, centrifuging at 8000 rpm to remove supernatant, alternately washing precipitate with ethanol and water for three times, and drying at 60 ℃ in a vacuum drying oven for 12 h to obtain the zinc oxide quantum dot.
The embodiment also provides a preparation method of the high-frequency transformer nanocrystalline magnetic core material, which comprises the following steps:
S1, mixing nanocrystalline soft magnetic powder, graphene quantum dots, zinc oxide quantum dots and dopamine in distilled water according to the mass parts, wherein the mass ratio of the distilled water to the nanocrystalline soft magnetic powder is 35: stirring at 1,500 rpm for 2h, regulating pH to 9 with 1 mol/L NaOH solution, stirring for 5h, filtering to remove supernatant, washing precipitate with distilled water for three times, and drying at 60deg.C in vacuum drying oven for 12h to obtain composite material;
s2, placing the composite material prepared in the step S1 into a vacuum smelting furnace, filling argon as protective gas until the air pressure is 400 mbar, performing heat treatment in a gradual heating mode, heating to 320 ℃ for the first time, and preserving heat for 15: 15 min; heating to 420 ℃ for the second time, and preserving heat for 15 min; heating to 520 ℃ for the third time, preserving heat 35 min, stirring 5min every 10: 10min, heating at 8 ℃/min, and cooling to room temperature at the speed of 10 ℃/min after heat treatment to obtain a heat treatment product;
And S3, placing the heat treatment product prepared in the step S2 into liquid nitrogen for cold treatment for 1 h, and recovering to room temperature to obtain the nanocrystalline magnetic core material.
Comparative example 1: this comparative example proposes a high frequency transformer nanocrystalline magnetic core material which differs from example 1 only in that no graphene quantum dots are added, and the remaining components, component contents, experimental steps are the same as example 1.
Comparative example 2: this comparative example proposes a high frequency transformer nanocrystalline core material which differs from example 1 only in that no zinc oxide quantum dots are added, and the remaining components, component contents, experimental steps are the same as example 1.
Comparative example 3: this comparative example proposes a nanocrystalline core material for a high frequency transformer, which differs from example 1 only in that no dopamine is added, and the remaining components, component contents, experimental procedures are the same as example 1.
Experimental example 1: the microscopic morphology of the nanocrystalline core material prepared in example 1 was observed using a scanning electron microscope.
FIG. 1 is a scanning electron microscope image of the nanocrystalline core material prepared in example 1 of this invention, where the nanocrystalline core material is spherical, has a small particle size, and slightly aggregates, indicating successful preparation of the nanocrystalline core material.
Experimental example 2: XRD patterns of the nanocrystalline magnetic core material and nanocrystalline soft magnetic powder prepared in example 1 were analyzed using an X-ray diffractometer.
Fig. 2 is an XRD pattern of the nanocrystalline magnetic core material and nanocrystalline soft magnetic powder prepared in example 1 of the present invention, where the XRD pattern of the nanocrystalline soft magnetic powder has no obvious diffraction peak, is amorphous powder, and after heat treatment together with graphene quantum dots, zinc oxide quantum dots and dopamine, the amorphous powder is recrystallized to eliminate residual stress in the rapid solidification process, and the synthesized nanocrystalline magnetic core material has an obvious diffraction peak, indicating successful preparation of nanocrystalline magnetic core material.
Experimental example 3: performance test:
The nanocrystalline core materials prepared in examples 1 to 3 and comparative examples 1 to 3 were placed in a mold and pressed into a toroidal core of 8mm ×4mm ×4mm (outer diameter×inner diameter×height), placed in an oven at 100 ℃ to cure and hold 10 h, and returned to room temperature, and the following performance tests were performed using a Vibrating Sample Magnetometer (VSM) and an impedance analyzer, and the performance data are shown in table 1.
TABLE 1 Performance test results
As shown in Table 1, the electromagnetic properties of examples 1-3 are superior to those of comparative examples 1-3, and have higher saturation magnetization and relative permeability, lower coercive force and lower hysteresis loss. The method shows that the graphene quantum dots, the zinc oxide quantum dots and the nanocrystalline soft magnetic powder are subjected to heat treatment together, so that the electromagnetic performance of the nanocrystalline magnetic core material is effectively improved, and meanwhile, the surface property of the material can be further optimized by adding dopamine and heating together, so that hysteresis loss is reduced.
Those of ordinary skill in the art will appreciate that: the discussion of any of the embodiments above is merely exemplary and is not intended to suggest that the scope of the invention (including the claims) is limited to these examples; the technical features of the above embodiments or in the different embodiments may also be combined within the idea of the invention, the steps may be implemented in any order and there are many other variations of the different aspects of the invention as described above, which are not provided in detail for the sake of brevity.
Claims (6)
1. The nanocrystalline magnetic core material of the high-frequency transformer is characterized by comprising the following synthetic raw materials in parts by weight: 60-80 parts of nanocrystalline soft magnetic powder with a molecular formula of Fe aSibBcXdCue, wherein X is one or more of Nb, co, mo, ce, a is more than or equal to 60 and less than or equal to 68, b is more than or equal to 10 and less than or equal to 15, c is more than or equal to 2 and less than or equal to 6, d is more than or equal to 4 and less than or equal to 6, e is more than or equal to 6 and less than or equal to 13, a+b+c+d+e=100, 10-20 parts of graphene quantum dots, 10-15 parts of zinc oxide quantum dots and 4-6 parts of dopamine;
The preparation method of the high-frequency transformer nanocrystalline magnetic core material comprises the following steps:
S1, mixing nanocrystalline soft magnetic powder, graphene quantum dots, zinc oxide quantum dots and dopamine in distilled water according to the mass parts, wherein the mass ratio of the distilled water to the nanocrystalline soft magnetic powder is 30-40: stirring at 1,460-560 rpm for 2h, regulating the pH to 9 by using 1 mol/L NaOH solution, continuously stirring for 4-6 hours, filtering to remove supernatant, washing the precipitate by using distilled water for three times, and drying at 60 ℃ in a vacuum drying oven for 12h to obtain a composite material;
S2, placing the composite material prepared in the step S1 into a vacuum smelting furnace, filling argon as protective gas until the air pressure is 300-500 mbar, performing heat treatment in a gradual heating mode, heating to 300-350 ℃ for the first time, and preserving heat for 10-20 min; heating to 400-450 ℃ for the second time, and preserving heat for 10-20 min; heating to 500-550 ℃ for the third time, preserving heat for 30-40 min, stirring for 5 min every 10min, heating at a speed of 8 ℃/min, and cooling to room temperature at a speed of 10 ℃/min after heat treatment is finished to obtain a heat treatment product;
And S3, placing the heat treatment product prepared in the step S2 into liquid nitrogen for cold treatment for 1 h, and recovering to room temperature to obtain the nanocrystalline magnetic core material.
2. The nanocrystalline magnetic core material for a high frequency transformer according to claim 1, wherein the method for preparing nanocrystalline soft magnetic powder comprises the steps of:
① . According to molecular formula of the nanocrystalline soft magnetic powder, weighing elementary substance raw materials of each element, adding the elementary substance raw materials into a vacuum smelting furnace, filling argon as protective gas until the air pressure is 300-500 mbar, and heating to 1400 ℃ to enable the elementary substance raw materials to be completely melted to obtain molten liquid;
② . Spraying the molten liquid prepared in the step ① onto a rotating cooling copper roller to obtain a nanocrystalline soft magnetic thin strip with a disordered structure, and mechanically crushing the nanocrystalline soft magnetic thin strip to obtain nanocrystalline soft magnetic powder.
3. The nanocrystalline magnetic core material for a high frequency transformer according to claim 2, wherein in the step ②, the distance between the nozzle and the cooling copper roller is 170-200 μm, and the rotational speed of the cooling copper roller is 20-40 m/s.
4. The high-frequency transformer nanocrystalline magnetic core material according to claim 3, wherein the preparation method of the graphene quantum dots comprises the following steps:
I. 200mg graphite oxide powder is weighed and dissolved in 100 mL distilled water, and is stirred at 460-560 rpm for 30min, 0.5 mL of 20 wt% ammonia water is added, and stirring is continued for 10min, so that a mixture is obtained;
and II, transferring the mixture prepared in the step I into a high-pressure reaction kettle with a polytetrafluoroethylene lining, heating for 6-8 h at 200 ℃, cooling to room temperature, alternately washing and precipitating for three times by using ethanol and water, and placing in a vacuum drying oven to dry at 60 ℃ for 12 h to obtain the graphene quantum dots.
5. The high-frequency transformer nanocrystalline magnetic core material according to claim 4, wherein the preparation method of the zinc oxide quantum dots comprises the following steps:
⑴ . Weighing 20 mM zinc salt, dissolving in 100mL ethanol, stirring and dissolving to synthesize zinc ion solution;
⑵ . Weighing 0.1-0.2 g of KOH and dissolving the KOH in 10 mL ethanol, and ultrasonically dissolving to synthesize an alkali solution;
⑶ . Dropwise adding the alkaline solution prepared in the step ⑵ into the zinc ion solution prepared in the step ⑴, stirring at 480-580 rpm, centrifuging to remove supernatant, alternately washing precipitate with ethanol and water for three times, and drying at 60 ℃ in a vacuum drying oven for 12h to obtain the zinc oxide quantum dot.
6. The nanocrystalline core material for a high frequency transformer according to claim 5, wherein in step ⑴, the zinc salt is any one of zinc chloride, zinc sulfate, zinc acetate, and zinc nitrate.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202410234244.XA CN117809925B (en) | 2024-03-01 | 2024-03-01 | Nanocrystalline magnetic core material of high-frequency transformer and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202410234244.XA CN117809925B (en) | 2024-03-01 | 2024-03-01 | Nanocrystalline magnetic core material of high-frequency transformer and preparation method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN117809925A CN117809925A (en) | 2024-04-02 |
CN117809925B true CN117809925B (en) | 2024-05-10 |
Family
ID=90426055
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202410234244.XA Active CN117809925B (en) | 2024-03-01 | 2024-03-01 | Nanocrystalline magnetic core material of high-frequency transformer and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN117809925B (en) |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103435829A (en) * | 2013-07-24 | 2013-12-11 | 烟台绿水赋膜材料有限公司 | Nanometer functionalization surface modification method based on o-dihydroxybenzene derivatives |
CN106582562A (en) * | 2015-10-20 | 2017-04-26 | 中国科学院大连化学物理研究所 | Magnetic graphene oxide composite nanomaterial and preparation method thereof |
CN112735724A (en) * | 2020-12-21 | 2021-04-30 | 安徽智磁新材料科技有限公司 | Iron-cobalt-based nanocrystalline magnetically soft alloy magnetic core material and preparation method thereof |
CN117430373A (en) * | 2023-12-21 | 2024-01-23 | 朗峰新材料启东有限公司 | Anti-interference nanocrystalline composite magnetic core material and preparation method thereof |
Family Cites Families (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7534489B2 (en) * | 2004-09-24 | 2009-05-19 | Agency For Science, Technology And Research | Coated composites of magnetic material and quantum dots |
-
2024
- 2024-03-01 CN CN202410234244.XA patent/CN117809925B/en active Active
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103435829A (en) * | 2013-07-24 | 2013-12-11 | 烟台绿水赋膜材料有限公司 | Nanometer functionalization surface modification method based on o-dihydroxybenzene derivatives |
CN106582562A (en) * | 2015-10-20 | 2017-04-26 | 中国科学院大连化学物理研究所 | Magnetic graphene oxide composite nanomaterial and preparation method thereof |
CN112735724A (en) * | 2020-12-21 | 2021-04-30 | 安徽智磁新材料科技有限公司 | Iron-cobalt-based nanocrystalline magnetically soft alloy magnetic core material and preparation method thereof |
CN117430373A (en) * | 2023-12-21 | 2024-01-23 | 朗峰新材料启东有限公司 | Anti-interference nanocrystalline composite magnetic core material and preparation method thereof |
Also Published As
Publication number | Publication date |
---|---|
CN117809925A (en) | 2024-04-02 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Liang et al. | SiC–Fe 3 O 4 dielectric–magnetic hybrid nanowires: controllable fabrication, characterization and electromagnetic wave absorption | |
CN112530655B (en) | Low-power-consumption soft magnetic alloy material and preparation method and application thereof | |
CN108377638A (en) | A kind of Co/C composite electromagnetics wave absorbing agent and preparation method thereof | |
CN111968821A (en) | Soft magnetic alloy powder and preparation method thereof, and magnetic ring inductor and preparation method thereof | |
JP6427061B2 (en) | Method of preparing core-shell-shell FeCo / SiO2 / MnBi nanoparticles, and core-shell-shell FeCo / SiO2 / MnBi nanoparticles | |
CN111554465A (en) | Nanocrystalline magnetically soft alloy and preparation method and application thereof | |
Li et al. | High frequency application of ultrafine submicron FeBP amorphous soft magnetic composites | |
Jiang et al. | A simple route to synthesize ZnFe2O4 hollow spheres and their magnetorheological characteristics | |
CN117637282A (en) | Corrosion-resistant iron-based nanocrystalline magnetically soft alloy and preparation method thereof | |
CN108723383B (en) | Controllable preparation method of multi-morphology iron-cobalt alloy magnetic nanoparticles with high saturation magnetic induction intensity | |
CN117809925B (en) | Nanocrystalline magnetic core material of high-frequency transformer and preparation method thereof | |
CN110783091B (en) | Preparation method of nanocrystalline FeSiBCr magnetic powder core | |
Tyagi et al. | Reaction kinetic, magnetic and microwave absorption studies of SrFe 12 O 19/CoFe 2 O 4 ferrite nanocrystals | |
CN109942026B (en) | Preparation method of monodisperse microporous nano-structured ferrite material | |
CN108461243B (en) | Porous camellia-shaped MnFe2O4@ C core-shell structure compound and preparation method thereof | |
CN112962024B (en) | Finemet-like Fe-based nanocrystalline magnetically soft alloy and preparation method thereof | |
Meng et al. | Nanocrystalline SrCe x Fe 12− x O 19 (x= 0.00, 0.02, 0.04, 0.06, 0.08) microfibers by sol–gel method | |
CN108511143A (en) | A kind of high-performance electromagnet | |
CN114496442A (en) | Nano magnetic particle, preparation method thereof and magnetic liquid | |
Yue et al. | Effect of Al-substitution on phase formation and magnetic properties of barium hexaferrite synthesized with sol-gel auto-combustion method | |
CN113025927A (en) | Iron-based amorphous composite material and preparation method and application thereof | |
CN105280320A (en) | Anisotropic high-frequency microwave magnetic material and preparation method thereof | |
JP2008254969A (en) | FLAKE LIKE IRON OXIDE PARTICULATE, FLAKE LIKE Fe BASE METAL PARTICULATE, AND METHOD FOR PRODUCING THEM | |
CN115608996B (en) | Iron-based nanocrystalline magnetically soft alloy powder and preparation method thereof | |
CN113214787B (en) | Wave-absorbing powder material and preparation method and application thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |