CN102212815A - Method for preparing ferroferric oxide coating on surface of iron-based amorphous strip by using high-temperature oxidation method - Google Patents

Method for preparing ferroferric oxide coating on surface of iron-based amorphous strip by using high-temperature oxidation method Download PDF

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CN102212815A
CN102212815A CN2011101660166A CN201110166016A CN102212815A CN 102212815 A CN102212815 A CN 102212815A CN 2011101660166 A CN2011101660166 A CN 2011101660166A CN 201110166016 A CN201110166016 A CN 201110166016A CN 102212815 A CN102212815 A CN 102212815A
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朱正吼
尹镭
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Nanchang University
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Abstract

The invention discloses a method for preparing a ferroferric oxide coating on the surface of an iron-based amorphous strip by using a high-temperature oxidation method. The method comprises the following steps of: (1) preparing raw materials; and (2) performing preparation: 1, preparing solute from NaOH, Na2CO3, Na3PO4.12H2O and Na2SiO3; 2, removing grease and oil; 3, performing ultrasonic treatment (the power of the ultrasonic is 1kw and the frequency of the ultrasonic is 40 kHz) for 10 to 15 minutes; 4, airing; 5, mixing solute consisting of NaOH and NaNO2 and solvent (namely deionized water) in a ratio of (500-700): (150-200); and 6, obtaining a film using Fe3O4 as a main component on the surface of the strip, wherein the thickness of the film is about 1 to 2 microns. The method has the advantages that: (1) the film using ferroferric oxide as the main component is formed on the surface of the oxidized iron-based amorphous strip, and the film has strong environment resistance and is not easily rusted; (2) the comprehensive soft magnetic performance of the oxidized iron-based amorphous strip is more excellent; and (3) the preparation process is simple and low in cost.

Description

A kind of high-temperature oxidation prepares the method for Z 250 coating in Fe-based amorphous strip surface
Technical field
The present invention relates to a kind of method for preparing the Z 250 coating, relate in particular to a kind of high-temperature oxidation prepares the Z 250 coating in Fe-based amorphous strip surface method.
Background technology
Along with the day of the energy is becoming tight and the deterioration of global environment, low-carbon energy-saving has become one of topic of paying close attention to the most in the whole world.In power electronic system, to soft magnetic materials research the becoming focus of energy-saving and environment friendly.Fe-based amorphous alloy band (the Fe that is developing at present 78Si 9B 13), Fe-based amorphous nanocrystalline alloy band (Fe 73.5Cu 1Nb 3Si 13.5B 9) because of its low-loss, high magnetic permeability, high saturated magnetic induction (Bs) become the most promising magnetically soft alloy material in the power system application, be Fe wherein with the ferrous alloy composition 78Si 9B 13, Fe 73.5Cu 1Nb 3Si 13.5B 9Become main flow, but the free surface activity of this material is not high, high frequency characteristics is lower, and its main component is iron, is easy in a humid environment get rusty and its outward appearance and performance are impacted.Thereby to develop surfactivity height, saturation induction density height, strong amorphous, the nanometer crystal alloy of opposing environment capacity, further improve its use properties and space.
Summary of the invention
The purpose of this invention is to provide a kind of high-temperature oxidation prepares the Z 250 coating in Fe-based amorphous strip surface method, Fe-based amorphous strip surface has formed the film of one deck based on Z 250 after oxidation, the ability of its opposing environment is strong, and contact resistance increases between the amorphous band.
The present invention is achieved in that step of preparation process is as follows: (1), starting material: Fe-based amorphous alloy band, strip width 0.5 ~ 220mm, thickness 20 ~ 50 μM; (2), preparation process: step 1: with NaOH, Na 2CO 3, Na 3PO 412H 2O, Na 2SiO 3Be solute, deionized water is a solvent, by volume (70 ~ 100): (30 ~ 50): (20 ~ 30): the ratio of (5 ~ 10), and configuration removes oil solution, and solution is heated to 80 ~ 90 ℃; Step 2: Fe-based amorphous band is put into the oil solution that removes that step 1 disposes, soak 10 ~ 30min at it and carry out degreasing degreasing; Step 3: it is to carry out ultrasonication 10-15min, ultrasonic power 1kw, frequency 40kHz in 80-95 ℃ the water-bath that the Fe-based amorphous band of step 2 gained is immersed in temperature; Step 4: the Fe-based amorphous band of step 3 gained is cleaned with distilled water, and then the HF with massfraction 5% carries out alligatoring to the surface of band, with the unnecessary acid solution of distilled water clean surface, dries; Step 5: with NaOH, NaNO 2Be solute, deionized water is a solvent, by volume (500 ~ 700): the ratio of (150 ~ 200), and the configuration oxidizing solution, and be heated to 130 ~ 150 ℃; Step 6: the Fe-based amorphous band of step 4 gained is immersed in the prepared oxidizing solution of step 5 fully, and oxidization time is 5 ~ 120min, obtains one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
The Fe-based amorphous alloy band is Fe 78Si 9B 13Or Fe 73.5Cu 1Nb 3Si 13.5B 9
Advantage of the present invention is: (1) Fe-based amorphous strip surface after oxidation has formed the film of one deck based on Z 250, and the ability of its opposing environment is strong, is difficult for getting rusty; (2) the comprehensive soft magnetic performance of Fe-based amorphous band is more excellent after the oxidation; (3) preparation technology is simple, and cost is low.
Description of drawings
Fig. 1 Fe 73.5Cu 1Nb 3Si 13.5B 9The XRD figure spectrum of former band of annealed state and surperficial high temperature oxidation band.
Fe after Fig. 2 oxidation 73.5Cu 1Nb 3Si 13.5B 9The SEM figure of amorphous nanocrystalline strip.
Embodiment
Embodiment 1:
Fe 73.5Cu 1Nb 3Si 13.5B 90.5 ~ 5mm is wide for the iron-based amorphous nanometer crystalline band, and 20 ~ 30 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 135 ℃ the oxidizing solution carries out oxide treatment 15min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 2:
Fe 73.5Cu 1Nb 3Si 13.5B 95 ~ 10mm is wide for the iron-based amorphous nanometer crystalline band, and 20 ~ 30 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 135 ℃ the oxidizing solution carries out oxide treatment 15min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 3:
Fe 73.5Cu 1Nb 3Si 13.5B 910 ~ 50mm is wide for the iron-based amorphous nanometer crystalline band, and 20 ~ 30 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 135 ℃ the oxidizing solution carries out oxide treatment 15min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 4:
Fe 73.5Cu 1Nb 3Si 13.5B 950 ~ 100mm is wide for the iron-based amorphous nanometer crystalline band, and 20 ~ 30 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 135 ℃ the oxidizing solution carries out oxide treatment 15min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 5:
Fe 73.5Cu 1Nb 3Si 13.5B 9100 ~ 150mm is wide for the iron-based amorphous nanometer crystalline band, and 20 ~ 30 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 135 ℃ the oxidizing solution carries out oxide treatment 15min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 6:
Fe 73.5Cu 1Nb 3Si 13.5B 9150 ~ 200mm is wide for the iron-based amorphous nanometer crystalline band, and 20 ~ 30 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 135 ℃ the oxidizing solution carries out oxide treatment 15min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 7:
Fe 73.5Cu 1Nb 3Si 13.5B 9200 ~ 220mm is wide for the iron-based amorphous nanometer crystalline band, and 20 ~ 30 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 135 ℃ the oxidizing solution carries out oxide treatment 15min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 8:
Fe 73.5Cu 1Nb 3Si 13.5B 95 ~ 10mm is wide for the iron-based amorphous nanometer crystalline band, and 30 ~ 40 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 135 ℃ the oxidizing solution carries out oxide treatment 15min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 9:
Fe 73.5Cu 1Nb 3Si 13.5B 9150 ~ 200mm is wide for the iron-based amorphous nanometer crystalline band, and 40 ~ 50 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 135 ℃ the oxidizing solution carries out oxide treatment 15min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 10:
Fe 73.5Cu 1Nb 3Si 13.5B 95 ~ 10mm is wide for the iron-based amorphous nanometer crystalline band, and 20 ~ 30 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 130 ℃ the oxidizing solution carries out oxide treatment 15min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 11:
Fe 73.5Cu 1Nb 3Si 13.5B 95 ~ 10mm is wide for the iron-based amorphous nanometer crystalline band, and 20 ~ 30 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 140 ℃ the oxidizing solution carries out oxide treatment 15min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 12:
Fe 73.5Cu 1Nb 3Si 13.5B 95 ~ 10mm is wide for the iron-based amorphous nanometer crystalline band, and 20 ~ 30 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 145 ℃ the oxidizing solution carries out oxide treatment 15min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 13:
Fe 73.5Cu 1Nb 3Si 13.5B 95 ~ 10mm is wide for the iron-based amorphous nanometer crystalline band, and 20 ~ 30 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 150 ℃ the oxidizing solution carries out oxide treatment 15min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 14:
Fe 73.5Cu 1Nb 3Si 13.5B 95 ~ 10mm is wide for the iron-based amorphous nanometer crystalline band, and 20 ~ 30 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 135 ℃ the oxidizing solution carries out oxide treatment 5min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 15:
Fe 73.5Cu 1Nb 3Si 13.5B 95 ~ 10mm is wide for the iron-based amorphous nanometer crystalline band, and 20 ~ 30 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 135 ℃ the oxidizing solution carries out oxide treatment 30min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 16:
Fe 73.5Cu 1Nb 3Si 13.5B 95 ~ 10mm is wide for the iron-based amorphous nanometer crystalline band, and 20 ~ 30 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 135 ℃ the oxidizing solution carries out oxide treatment 60min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 17:
Fe 73.5Cu 1Nb 3Si 13.5B 95 ~ 10mm is wide for the iron-based amorphous nanometer crystalline band, and 20 ~ 30 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 135 ℃ the oxidizing solution carries out oxide treatment 90min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 18:
Fe 73.5Cu 1Nb 3Si 13.5B 95 ~ 10mm is wide for the iron-based amorphous nanometer crystalline band, and 20 ~ 30 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 135 ℃ the oxidizing solution carries out oxide treatment 120min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Embodiment 19:
Fe 78Si 9B 13Fe-based amorphous band 5 ~ 10mm is wide, and 20 ~ 30 μM is thick, through 80 ~ 90 ℃ remove the oil solution oil removing after, it is immersed in 135 ℃ the oxidizing solution carries out oxide treatment 15min, obtain one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
Fe-based amorphous, iron-based amorphous nanometer crystalline band after handling are passed through XRD, and SEM carries out thing phase and Micro-Structure Analysis to it, tests its soft magnetic performance with MATS-2010SD soft magnetism DC test instrument.The result is as follows:
(1) Fe 73.5Cu 1Nb 3Si 13.5B 9The band material phase analysis
Fig. 1 is Fe 73.5Cu 1Nb 3Si 13.5B 9The XRD figure spectrum of former band of annealed state and surperficial high temperature oxidation band.From figure as can be known, Fe 73.5Cu 1Nb 3Si 13.5B 9The diffraction curve of annealed state band is 2
Figure 2011101660166100002DEST_PATH_IMAGE002
Be to occur tangible sharp peak near 44.8 °, 65.1 ° and 82.3 °, have tangible crystallization phase in this explanation band, be mainly Fe(Im-3m) phase.After the annealed state band carried out high temperature oxidation, strip surface generated Fe 3O 4Phase, and Fe is arranged 2O 3Exist mutually ,Its major cause is the Fe that generates 3O 4In a humid environment easily and due to the atmospheric oxidation.
(2) SEM of band observes behind the high temperature oxidation
As seen from Figure 2, strip surface has formed thickness and has been about 1-2 behind high temperature oxidation μThe film of m, because amorphous band is immersed in the alkali lye, the regional oxidizing reaction that surfactivity is big is stronger, causes the uneven of strip surface film after the oxidation.
(3) oxidation is to the influence of band soft magnetic performance
The main related data of table 1 magnetic hysteresis loop
Figure 2011101660166100002DEST_PATH_IMAGE004
As can be drawn from Table 1, the comprehensive soft magnetic performance of band increases behind high temperature oxidation.

Claims (2)

1. a high-temperature oxidation prepares the method for Z 250 coating in Fe-based amorphous strip surface, it is characterized in that step of preparation process is as follows: (1), starting material: Fe-based amorphous alloy band, strip width 0.5 ~ 220mm, thickness 20 ~ 50 μM; (2), preparation process: step 1: with NaOH, Na 2CO 3, Na 3PO 412H 2O, Na 2SiO 3Be solute, deionized water is a solvent, by volume (70 ~ 100): (30 ~ 50): (20 ~ 30): the ratio of (5 ~ 10), and configuration removes oil solution, and solution is heated to 80 ~ 90 ℃; Step 2: Fe-based amorphous band is put into the oil solution that removes that step 1 disposes, soak 10 ~ 30min at it and carry out degreasing degreasing; Step 3: it is to carry out ultrasonication 10-15min, ultrasonic power 1kw, frequency 40kHz in 80-95 ℃ the water-bath that the Fe-based amorphous band of step 2 gained is immersed in temperature; Step 4: the Fe-based amorphous band of step 3 gained is cleaned with distilled water, and then the HF with massfraction 5% carries out alligatoring to the surface of band, with the unnecessary acid solution of distilled water clean surface, dries; Step 5: with NaOH, NaNO 2Be solute, deionized water is a solvent, by volume (500 ~ 700): the ratio of (150 ~ 200), and the configuration oxidizing solution, and be heated to 130 ~ 150 ℃; Step 6: the Fe-based amorphous band of step 4 gained is immersed in the prepared oxidizing solution of step 5 fully, and oxidization time is 5 ~ 120min, obtains one deck with Fe in strip surface 3O 4Be main, the about 1-2 of thickness μThe film of m.
2. a kind of high-temperature oxidation according to claim 1 prepares the method for Z 250 coating in Fe-based amorphous strip surface, it is characterized in that the Fe-based amorphous alloy band is Fe 78Si 9B 13Or Fe 73.5Cu 1Nb 3Si 13.5B 9
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CN104465004A (en) * 2014-11-25 2015-03-25 浙江大学 Method for manufacturing high-saturation-flux-density soft magnetic composite material according to alkaline bluing technique
CN105695845A (en) * 2016-02-18 2016-06-22 南昌大学 Preparation process of heat dissipation and abrasion resistance material
CN111515578A (en) * 2019-02-04 2020-08-11 林肯环球股份有限公司 Coated welding wire
CN111850534A (en) * 2020-06-16 2020-10-30 中国石油天然气集团有限公司 Martensite stainless steel oil pipe low-stress pre-passivation film and preparation method thereof
WO2022134404A1 (en) * 2020-12-22 2022-06-30 横店集团东磁股份有限公司 Modified nanocrystalline strip, preparation method therefor, and application thereof
CN115094408A (en) * 2022-06-27 2022-09-23 黑龙江北方工具有限公司 Oxidation processing method for iron-based alloy parts

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104465004A (en) * 2014-11-25 2015-03-25 浙江大学 Method for manufacturing high-saturation-flux-density soft magnetic composite material according to alkaline bluing technique
CN105695845A (en) * 2016-02-18 2016-06-22 南昌大学 Preparation process of heat dissipation and abrasion resistance material
CN111515578A (en) * 2019-02-04 2020-08-11 林肯环球股份有限公司 Coated welding wire
CN111850534A (en) * 2020-06-16 2020-10-30 中国石油天然气集团有限公司 Martensite stainless steel oil pipe low-stress pre-passivation film and preparation method thereof
CN111850534B (en) * 2020-06-16 2022-03-01 中国石油天然气集团有限公司 Martensite stainless steel oil pipe low-stress pre-passivation film and preparation method thereof
WO2022134404A1 (en) * 2020-12-22 2022-06-30 横店集团东磁股份有限公司 Modified nanocrystalline strip, preparation method therefor, and application thereof
CN115094408A (en) * 2022-06-27 2022-09-23 黑龙江北方工具有限公司 Oxidation processing method for iron-based alloy parts

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