CN103436943B - A kind of Nano-composite Electrodeposition technology that utilizes is to the method for oriented silicon steel nitriding - Google Patents
A kind of Nano-composite Electrodeposition technology that utilizes is to the method for oriented silicon steel nitriding Download PDFInfo
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- CN103436943B CN103436943B CN201310348135.2A CN201310348135A CN103436943B CN 103436943 B CN103436943 B CN 103436943B CN 201310348135 A CN201310348135 A CN 201310348135A CN 103436943 B CN103436943 B CN 103436943B
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- silicon steel
- nano
- plating solution
- oriented silicon
- composite electrodeposition
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- 229910000976 Electrical steel Inorganic materials 0.000 title claims abstract description 40
- 238000005516 engineering process Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 20
- 238000005121 nitriding Methods 0.000 title claims abstract description 18
- 238000004070 electrodeposition Methods 0.000 title claims abstract description 14
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 12
- 238000007747 plating Methods 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000012153 distilled water Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 238000002791 soaking Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 5
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000007669 thermal treatment Methods 0.000 claims description 5
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- 239000002131 composite material Substances 0.000 abstract description 8
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 229910000831 Steel Inorganic materials 0.000 description 9
- 239000010959 steel Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 7
- 238000001953 recrystallisation Methods 0.000 description 6
- 238000000137 annealing Methods 0.000 description 3
- 238000004140 cleaning Methods 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 239000003112 inhibitor Substances 0.000 description 3
- 239000012669 liquid formulation Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000009628 steelmaking Methods 0.000 description 1
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- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
Abstract
The present invention relates to a kind of Nano-composite Electrodeposition technology that utilizes to the method for oriented silicon steel nitriding, comprise the following steps: 1) take each component by plating solution composition, drip hydrochloric acid, adjusted to ph is to 2.5-3.1; 2) by plating solution ultrasonic disperse in step 1) 30 minutes, re-use electric mixer and stir, by plating solution heating in water bath to 40 DEG C; 3) silicon steel sheet is cleaned up, select 10-30A/dm
2current density put into immediately through step 2) plating solution electroplate, after 3-5 minute take out, with distilled water clean after naturally dry; And 4) silicon steel sheet through step 3) is put into gas shield stove, heat-treat, soaking time is 2 hours.Beneficial effect of the present invention is: the technology adopting composite electrodeposition, simultaneously combining nano technology and heat-treating methods, and at a lower temperature, at oriented silicon steel surface carburization, technique relative ease, has very high economic worth.
Description
Technical field
The present invention relates to oriented silicon steel technical field, particularly relate to a kind of Nano-composite Electrodeposition technology that utilizes to the method for oriented silicon steel nitriding.
Background technology
Oriented silicon steel has good magnetic property and very low iron loss, is to manufacture the essential material of transformer core, and annual consumption reaches millions of tons, and the manufacturing process of oriented silicon steel is complicated, manufacturing process head and to affect performance factor many.The great demand amount of oriented silicon steel and improving constantly its performance, make scientific workers to the research of silicon steel constantly dark people.
Usually, the recrystallization annealing of oriented silicon steel comprises primary recrystallization annealing and secondary recrystallization annealing, the texture that silicon steel is final and tissue are formed by secondary recrystallization, but the texture of primary recrystallization has important impact to the tissue of secondary recrystallization and texture.All very clear in the formation mechenism of oriented silicon steel texture is not all at present, also need the research of some originality.Such as some think that coincidence site lattice plays a key effect in goss texture forming process, but also someone thinks having the greatest impact of high energy crystal boundary.So the research about oriented silicon steel recrystallize also needs 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, investigator is absorbed in the research of low temperature manufacturing process mostly.The technology that low temperature manufactures, can make inhibitor not only be formed by addition element in steelmaking process, also can be formed in the course of processing, adopt nitridation technique to be one of them very important research direction.
Current nitridation technique, main limitation is, 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 of infiltrating concentrates on the interface of material, inhibitor distributes very uneven in a thickness direction, and the surperficial N of steel plate is easy to get back in atmosphere simultaneously, finally makes the N element content of surface of steel plate very unstable, and product performance fluctuation is very large.
Summary of the invention
The object of this invention is to provide a kind of Nano-composite Electrodeposition technology that utilizes to the method for oriented silicon steel nitriding, to overcome currently available technology above shortcomings.
The object of the invention is to be achieved through the following technical solutions:
Utilize Nano-composite Electrodeposition technology to a method for oriented silicon steel nitriding, comprise the following steps:
1) take each component by plating solution composition, drip hydrochloric acid, adjusted to ph is to 2.5-3.1, and 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; Nano-aluminum nitride: 5-25g/L, surplus is water, and above each component is analytical pure;
2) by plating solution ultrasonic disperse in step 1) 30 minutes, re-use electric mixer and stir, by plating solution heating in water bath to 40 DEG C;
3) silicon steel sheet is cleaned up, select 10-30A/dm
2current density put into immediately through step 2) plating solution electroplate, after 3-5 minute take out, with distilled water clean after naturally dry; And
4) silicon steel sheet through step 3) is put into gas shield stove, heat-treat, soaking time is 2 hours.
Further, the hydrochloric acid of hydrochloric acid to be volume ratio be 1:1 in described step 1).
Further, described step 2) in agitator speed be 200-400 rev/min.
Further, in described step 4), gas shield stove is nitrogen: hydrogen is the gas shield stove of 1:3.
Further, in described step 4), thermal treatment temp is set to 600-800 DEG C.
Further, described nano-aluminum nitride particle diameter is 50nm.
Beneficial effect of the present invention is: the technology adopting composite electrodeposition, simultaneously combining nano technology and heat-treating methods, and at a lower temperature, at oriented silicon steel surface carburization, technique relative ease, has 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; Nano-aluminum nitride: 5g/L, surplus is water, and above each component is analytical pure, and nano-aluminum nitride particle diameter is about 50nm;
(2) by above formula, take medicine, add distilled water mixed dissolution; Dripping volume ratio is the hydrochloric acid of 1:1, adjusted to ph to 2.5;
(3) by above plating solution ultrasonic disperse 30 minutes, re-use electric mixer and stir, rotating speed is set to 200 revs/min, by plating solution heating in water bath to 40 DEG C;
(4) silicon steel sheet is cleaned up, select 10A/dm
2current density put into plating solution immediately and electroplate; Electroplate after 5 minutes and take out, naturally dry after cleaning with distilled water; Finally on steel plate, generate Fe-AlN composite deposite;
(5) silicon steel sheet being coated with Fe-AlN composite deposite is above put into nitrogen: hydrogen is the gas shield stove of 1:3, heat-treats, and thermal treatment temp is set to 600 DEG C, soaking time is 2 hours.
Test the silicon steel steel plate obtained, 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; Nano-aluminum nitride: 15g/L, surplus is water, and above each component is analytical pure, and nano-aluminum nitride particle diameter is about 50nm;
(2) by above formula, take medicine, add distilled water mixed dissolution; Dripping volume ratio is the hydrochloric acid of 1:1, adjusted to ph to 2.8;
(3) by above plating solution ultrasonic disperse 30 minutes, re-use electric mixer and stir, rotating speed is set to 300 revs/min, by plating solution heating in water bath to 40 DEG C;
(4) silicon steel sheet is cleaned up, select 20A/dm
2current density put into plating solution immediately and electroplate; Electroplate after 5 minutes and take out, naturally dry after cleaning with distilled water; Finally on steel plate, generate Fe-AlN composite deposite;
(5) silicon steel sheet being coated with Fe-AlN composite deposite is above put into nitrogen: hydrogen is the gas shield stove of 1:3, heat-treats, and thermal treatment temp is set to 700 DEG C, soaking time is 2 hours.
Test the silicon steel steel plate obtained, 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; Nano-aluminum nitride: 25g/L, surplus is water, and above each component is analytical pure, and nano-aluminum nitride particle diameter is about 50nm;
(2) by above formula, take medicine, add distilled water mixed dissolution; Dripping volume ratio is the hydrochloric acid of 1:1, adjusted to ph to 3.1;
(3) by above plating solution ultrasonic disperse 30 minutes, re-use electric mixer and stir, rotating speed is set to 400 revs/min, by plating solution heating in water bath to 40 DEG C;
(4) silicon steel sheet is cleaned up, select 30A/dm
2current density put into plating solution immediately and electroplate; Electroplate after 5 minutes and take out, naturally dry after cleaning with distilled water; Finally on steel plate, generate Fe-AlN composite deposite;
(5) silicon steel sheet being coated with Fe-AlN composite deposite is above put into nitrogen: hydrogen is the gas shield stove of 1:3, heat-treats, and thermal treatment temp is set to 800 DEG C, soaking time is 2 hours.
Test the silicon steel steel plate obtained, 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 any change is done in its shape or structure; every have identical with the application or akin technical scheme, all drops within protection scope of the present invention.
Claims (6)
1. utilize Nano-composite Electrodeposition technology to a method for oriented silicon steel nitriding, it is characterized in that, comprise the following steps:
1) take each component by plating solution composition, drip hydrochloric acid, adjusted to ph is to 2.5-3.1, and 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; Nano-aluminum nitride: 5-25g/L, surplus is water, and above each component is analytical pure;
2) by plating solution ultrasonic disperse in step 1) 30 minutes, re-use electric mixer and stir, by plating solution heating in water bath to 40 DEG C;
3) silicon steel sheet is cleaned up, select 10-30A/dm
2current density put into immediately through step 2) plating solution electroplate, after 3-5 minute take out, with distilled water clean after naturally dry; And
4) silicon steel sheet through step 3) is put into gas shield stove, heat-treat, soaking time is 2 hours.
2. the Nano-composite Electrodeposition technology that utilizes according to claim 1 is to the method for oriented silicon steel nitriding, it is characterized in that: described nano-aluminum nitride particle diameter is 50nm.
3. the Nano-composite Electrodeposition technology that utilizes according to claim 1 is to the method for oriented silicon steel nitriding, it is characterized in that: in described step 1), and described hydrochloric acid is the hydrochloric acid soln mixed with water by the volume ratio of 1:1.
4. the Nano-composite Electrodeposition technology that utilizes according to claim 3 is to the method for oriented silicon steel nitriding, it is characterized in that: described step 2) in, agitator speed is 200-400 rev/min.
5. the Nano-composite Electrodeposition technology that utilizes according to claim 4 is to the method for oriented silicon steel nitriding, it is characterized in that: in described step 4), and gas shield stove is nitrogen: hydrogen is the gas shield stove of 1:3.
6. the Nano-composite Electrodeposition technology that utilizes according to claim 5 is to the method for oriented silicon steel nitriding, it is characterized in that: in described step 4), thermal treatment temp is set to 600-800 DEG C.
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| CN103436943B true CN103436943B (en) | 2016-01-20 |
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| CN106702466B (en) * | 2017-03-10 | 2019-02-26 | 武汉科技大学 | A kind of high magnetic high silicon electrical steel and preparation 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 |
| 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 |
Citations (2)
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|---|---|---|---|---|
| DE102005040151A1 (en) * | 2005-08-25 | 2007-03-01 | Galvotech Dier Gmbh | Electrodeposition of metal coatings, preferably Ni or Cu, from electrolyte solutions containing hard particles, e.g. of corundum useful for ingot mold plates and continuous casting molds |
| CN101532150A (en) * | 2009-04-14 | 2009-09-16 | 合肥工业大学 | Acid copper-aluminium nitride high-performance composite coating plating solution and coating method thereof |
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| KR100333440B1 (en) * | 1999-12-31 | 2002-04-25 | 허 태 학 | Strain for disintegrating gasoline Pseudomonas sp. HPLG-1 |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102005040151A1 (en) * | 2005-08-25 | 2007-03-01 | Galvotech Dier Gmbh | Electrodeposition of metal coatings, preferably Ni or Cu, from electrolyte solutions containing hard particles, e.g. of corundum useful for ingot mold plates and continuous casting molds |
| CN101532150A (en) * | 2009-04-14 | 2009-09-16 | 合肥工业大学 | Acid copper-aluminium nitride high-performance composite coating plating solution and coating method thereof |
Non-Patent Citations (3)
| Title |
|---|
| Microstructures of Ni-AlN composite coatings prepared by pulse electrodeposition technology;Fafeng Xia等;《Applied Surface Science》;20121220;第7-11页 * |
| 抗坏血酸在电沉积铁中的应用;李超群等;《电镀与精饰》;20080115;第30卷(第1期);第3-7页 * |
| 电沉积Cu一纳米A1N复合涂层的耐腐蚀性研究;李鹏等;《金属功能材料》;20100815;第17卷(第4期);第38-40页 * |
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