CN103436943A - Method for nitriding oriented silicon steel by adopting nano-composite electrodeposition technology - Google Patents

Method for nitriding oriented silicon steel by adopting nano-composite electrodeposition technology Download PDF

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CN103436943A
CN103436943A CN2013103481352A CN201310348135A CN103436943A CN 103436943 A CN103436943 A CN 103436943A CN 2013103481352 A CN2013103481352 A CN 2013103481352A CN 201310348135 A CN201310348135 A CN 201310348135A CN 103436943 A CN103436943 A CN 103436943A
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silicon steel
plating solution
nano
oriented silicon
composite electrodeposition
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CN103436943B (en
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张洁清
赵仁南
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WUXI GUANGXU NEW MATERIAL TECHNOLOGY Co Ltd
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WUXI GUANGXU NEW MATERIAL TECHNOLOGY Co Ltd
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Abstract

The invention relates to a method for nitriding oriented silicon steel by adopting the nano-composite electrodeposition technology, which comprises the following steps: 1) weighing all components as per the composition of a plating solution, dropwise adding hydrochloric acid, and adjusting the pH value to be 2.5-3.1; 2) dispersing the plating solution obtained in the step 1) for 30 minutes, then agitating with an electric agitator, and heating the plating solution in water bath to 40 DEG C; 3) cleaning a silicon steel plate through washing, placing the silicon steel plate into the plating solution obtained in the step 2) for electroplating under the electric current density of 10-30A/dm2, taking out the silicon steel plate after 3-5 minutes, cleaning the silicon steel plate with distilled water, and air drying the silicon steel plate; 4) placing the silicon steel plate from the step 3) into an atmosphere furnace for heat treatment, and keeping the temperature for 2 hours. The method has the benefits as follows: the nano-composite electrodeposition technology is adopted, and the method integrates nanometer technology and heat treatment at the same time, so that the surface of the oriented silicon steel can be nitrided under the low temperature, the process is relatively simple and convenient, and high economic value can be achieved.

Description

A kind of method of Nano-composite Electrodeposition technology to the oriented silicon steel nitriding of utilizing
Technical field
The present invention relates to the oriented silicon steel technical field, relate in particular to a kind of method of Nano-composite Electrodeposition technology to the oriented silicon steel nitriding of utilizing.
Background technology
Oriented silicon steel has good magnetic property and very low iron loss, is the essential material of manufacturing transformer core, and annual consumption reaches millions of tons, the manufacturing process complexity of oriented silicon steel, manufacturing process head and to affect performance factor many.The great demand amount of oriented silicon steel and to the improving constantly of its performance, make scientific workers to the constantly dark people of the research of silicon steel.
Usually, the recrystallization annealing of oriented silicon steel comprises primary recrystallization annealing and secondary recrystallization annealing, the final texture of silicon steel and tissue form by secondary recrystallization, but the texture of primary recrystallization has important impact to tissue and the texture of secondary recrystallization.At present all very clear about the not all aspect of formation mechanism of oriented silicon steel texture, also need the research of some originality.Such as some think in the goss texture forming process that coincidence site lattice plays a key effect, but also someone thinks having the greatest impact of high energy crystal boundary.So, about the research of oriented silicon steel recrystallize, also need to do a lot of work.
The manufacturing technology of oriented silicon steel is divided into high temperature manufacturing process and low temperature manufacturing process.At present, because energy consumption is too large, the investigator is absorbed in the research of low temperature manufacturing process mostly.The technology that low temperature is manufactured can also can form so that inhibitor not only forms by addition element in steelmaking process in the course of processing, and adopting nitridation technique is one of them very important research direction.
Current nitridation technique, main limitation is, and the efficiency of nitriding is very low, and the temperature of nitriding is still very high, and energy consumption is very large.Simultaneously in nitriding process, very large to the damage of nitriding equipment.Because the N element infiltrated concentrates on the interface of material, inhibitor distributes very inhomogeneous on thickness direction, and the surperficial N of steel plate is easy to get back in atmosphere simultaneously, finally makes the N constituent content of surface of steel plate very unstable, and the product performance fluctuation is very large.
Summary of the invention
The purpose of this invention is to provide a kind of method of Nano-composite Electrodeposition technology to the oriented silicon steel nitriding of utilizing, to overcome the currently available technology above shortcomings.
The objective of the invention is to be achieved through the following technical solutions:
A kind of method of Nano-composite Electrodeposition technology to the oriented silicon steel nitriding of utilizing comprises the following steps:
1) form and take each component by plating solution, drip hydrochloric acid, adjust the pH value to 2.5-3.1, plating solution used is composed of the following components: FeSO 46H 2o:200-250g/L; FeCl 26H 2o:35-45g/L; H 3bO 3: 35-40g/L; Cetyl trimethylammonium bromide: 0.1-0.3g/L; Xitix: 3-5g/L; Nanometer AlN:5-25g/L, surplus is water, above each component is analytical pure;
2), by the ultrasonic dispersion of plating solution in step 1) 30 minutes, re-use electric mixer and stir, by plating solution heating in water bath to 40 ℃;
3) silicon steel sheet is cleaned up, select 10-30A/dm 2current density put into through step 2 immediately) plating solution electroplate, after 3-5 minute, take out, after cleaning with distilled water, naturally dry; And
4) will put into the gas shield stove through the silicon steel sheet of step 3), and heat-treat, soaking time is 2 hours.
Further, in described step 1), hydrochloric acid is the hydrochloric acid that volume ratio is 1:1.
Further, described step 2), agitator speed is 200-400 rev/min.
Further, in described step 4), the gas shield stove is nitrogen: the gas shield stove that hydrogen is 1:3.
Further, in described step 4), thermal treatment temp is set to 600-800 ℃.
Further, described nanometer AlN particle diameter is 50nm.
Beneficial effect of the present invention is: adopt the technology of composite electrodeposition, and while combining nano technology and heat-treating methods, at lower temperature, at the oriented silicon steel surface carburization, the technique relative simple, have very high economic worth.
Embodiment
Embodiment 1:
(1) electroplate liquid formulation: FeSO 46H 2o:200g/L; FeCl 26H 2o:35g/L; H 3bO 3: 35g/L; Cetyl trimethylammonium bromide: 0.1g/L; Xitix: 3g/L; Nanometer AlN:5g/L, surplus is water, above each component is analytical pure, the about 50nm of nanometer AlN particle diameter;
(2) by above formula, take medicine, add the distilled water mixed dissolution; The hydrochloric acid that the dropping volume ratio is 1:1, adjust pH value to 2.5;
(3) by the ultrasonic dispersion of above plating solution 30 minutes, re-use electric mixer and stir, rotating speed is set to 200 rev/mins, by plating solution heating in water bath to 40 ℃;
(4) silicon steel sheet is cleaned up, select 10A/dm 2current density put into immediately plating solution and electroplate; Electroplate after 5 minutes and take out, naturally dry after cleaning with distilled water; Finally on steel plate, generate the Fe-AlN composite deposite;
(5) silicon steel sheet that is coated with the Fe-AlN composite deposite more than general is put into nitrogen: the gas shield stove that hydrogen is 1:3, to heat-treat, and thermal treatment temp is set to 600 ℃, and soaking time is 2 hours.
The silicon steel steel plate obtained is tested, and the results are shown in Table 1.
Embodiment 2:
(1) electroplate liquid formulation: FeSO 46H 2o:220g/L; FeCl 26H 2o:40g/L; H 3bO 3: 38g/L; Cetyl trimethylammonium bromide: 0.2g/L; Xitix: 4g/L; Nanometer AlN:15g/L, surplus is water, above each component is analytical pure, the about 50nm of nanometer AlN particle diameter;
(2) by above formula, take medicine, add the distilled water mixed dissolution; The hydrochloric acid that the dropping volume ratio is 1:1, adjust pH value to 2.8;
(3) by the ultrasonic dispersion of above plating solution 30 minutes, re-use electric mixer and stir, rotating speed is set to 300 rev/mins, by plating solution heating in water bath to 40 ℃;
(4) silicon steel sheet is cleaned up, select 20A/dm 2current density put into immediately plating solution and electroplate; Electroplate after 5 minutes and take out, naturally dry after cleaning with distilled water; Finally on steel plate, generate the Fe-AlN composite deposite;
(5) silicon steel sheet that is coated with the Fe-AlN composite deposite more than general is put into nitrogen: the gas shield stove that hydrogen is 1:3, to heat-treat, and thermal treatment temp is set to 700 ℃, and soaking time is 2 hours.
The silicon steel steel plate obtained is tested, and the results are shown in Table 1.
Embodiment 3:
(1) electroplate liquid formulation: FeSO 46H 2o:250g/L; FeCl 26H 2o:45g/L; H 3bO 3: 40g/L; Cetyl trimethylammonium bromide: 0.3g/L; Xitix: 5g/L; Nanometer AlN:25g/L, surplus is water, above each component is analytical pure, the about 50nm of nanometer AlN particle diameter;
(2) by above formula, take medicine, add the distilled water mixed dissolution; The hydrochloric acid that the dropping volume ratio is 1:1, adjust pH value to 3.1;
(3) by the ultrasonic dispersion of above plating solution 30 minutes, re-use electric mixer and stir, rotating speed is set to 400 rev/mins, by plating solution heating in water bath to 40 ℃;
(4) silicon steel sheet is cleaned up, select 30A/dm 2current density put into immediately plating solution and electroplate; Electroplate after 5 minutes and take out, naturally dry after cleaning with distilled water; Finally on steel plate, generate the Fe-AlN composite deposite;
(5) silicon steel sheet that is coated with the Fe-AlN composite deposite more than general is put into nitrogen: the gas shield stove that hydrogen is 1:3, to heat-treat, and thermal treatment temp is set to 800 ℃, and soaking time is 2 hours.
The silicon steel steel plate obtained is tested, and the results are shown in Table 1.
Nitriding silicon steel steel plate test result prepared by the present invention:
? Embodiment 1 Embodiment 2 Embodiment 3
Nitriding amount (ppm) 200 180 110
Inhibitor mean sizes (nm) 89 67 53
B 8(T) 1.82 1.81 1.83
The present invention is not limited to above-mentioned preferred forms; anyone can draw other various forms of products under enlightenment of the present invention; no matter but do any variation on its shape or structure; every have identical with a application or akin technical scheme, within all dropping on protection scope of the present invention.

Claims (6)

1. one kind is utilized the method for Nano-composite Electrodeposition technology to the oriented silicon steel nitriding, it is characterized in that, comprises the following steps:
1) form and take each component by plating solution, drip hydrochloric acid, adjust the pH value to 2.5-3.1, plating solution used is composed of the following components: FeSO 46H 2o:200-250g/L; FeCl 26H 2o:35-45g/L; H 3bO 3: 35-40g/L; Cetyl trimethylammonium bromide: 0.1-0.3g/L; Xitix: 3-5g/L; Nanometer AlN:5-25g/L, surplus is water, above each component is analytical pure;
2), by the ultrasonic dispersion of plating solution in step 1) 30 minutes, re-use electric mixer and stir, by plating solution heating in water bath to 40 ℃;
3) silicon steel sheet is cleaned up, select 10-30A/dm 2current density put into through step 2 immediately) plating solution electroplate, after 3-5 minute, take out, after cleaning with distilled water, naturally dry; And
4) will put into the gas shield stove through the silicon steel sheet of step 3), and heat-treat, soaking time is 2 hours.
2. the method for Nano-composite Electrodeposition technology to the oriented silicon steel nitriding of utilizing according to claim 1, it is characterized in that: described nanometer AlN particle diameter is 50nm.
3. the method for Nano-composite Electrodeposition technology to the oriented silicon steel nitriding of utilizing according to claim 1, it is characterized in that: in described step 1), hydrochloric acid is the hydrochloric acid that volume ratio is 1:1.
4. the method for Nano-composite Electrodeposition technology to the oriented silicon steel nitriding of utilizing according to claim 3, it is characterized in that: described step 2), agitator speed is 200-400 rev/min.
5. the method for Nano-composite Electrodeposition technology to the oriented silicon steel nitriding of utilizing according to claim 4, it is characterized in that: in described step 4), the gas shield stove is nitrogen: the gas shield stove that hydrogen is 1:3.
6. the method for Nano-composite Electrodeposition technology to the oriented silicon steel nitriding of utilizing according to claim 5, it is characterized in that: in described step 4), thermal treatment temp is set to 600-800 ℃.
CN201310348135.2A 2013-08-12 2013-08-12 A kind of Nano-composite Electrodeposition technology that utilizes is to the method for oriented silicon steel nitriding Active CN103436943B (en)

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CN106702466A (en) * 2017-03-10 2017-05-24 武汉科技大学 High-magnetism high-silicon electrical steel and preparing method thereof
CN111826654A (en) * 2020-07-06 2020-10-27 安徽省赛威输送设备有限公司 Processing method for improving corrosion resistance of elevator shell
CN115354272A (en) * 2022-07-21 2022-11-18 江苏甬金金属科技有限公司 Corrosion-resistant stainless steel band and processing technology thereof

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CN111826654A (en) * 2020-07-06 2020-10-27 安徽省赛威输送设备有限公司 Processing method for improving corrosion resistance of elevator shell
CN115354272A (en) * 2022-07-21 2022-11-18 江苏甬金金属科技有限公司 Corrosion-resistant stainless steel band and processing technology thereof
CN115354272B (en) * 2022-07-21 2024-02-02 江苏甬金金属科技有限公司 Corrosion-resistant stainless steel belt and processing technology thereof

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