CN105220194A - A kind of method for electroplating nickel of neodymium iron boron thin slice magnet steel product - Google Patents
A kind of method for electroplating nickel of neodymium iron boron thin slice magnet steel product Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 252
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 126
- 229910001172 neodymium magnet Inorganic materials 0.000 title claims abstract description 124
- 238000000034 method Methods 0.000 title claims abstract description 66
- 229910000831 Steel Inorganic materials 0.000 title claims abstract description 43
- 239000010959 steel Substances 0.000 title claims abstract description 43
- 238000009713 electroplating Methods 0.000 title claims abstract description 24
- QJVKUMXDEUEQLH-UHFFFAOYSA-N [B].[Fe].[Nd] Chemical compound [B].[Fe].[Nd] QJVKUMXDEUEQLH-UHFFFAOYSA-N 0.000 title claims description 9
- 238000007747 plating Methods 0.000 claims abstract description 66
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000004327 boric acid Substances 0.000 claims abstract description 33
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims abstract description 31
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims abstract description 31
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims abstract description 20
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims abstract description 20
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims abstract description 14
- 235000011130 ammonium sulphate Nutrition 0.000 claims abstract description 14
- LJCNRYVRMXRIQR-OLXYHTOASA-L potassium sodium L-tartrate Chemical compound [Na+].[K+].[O-]C(=O)[C@H](O)[C@@H](O)C([O-])=O LJCNRYVRMXRIQR-OLXYHTOASA-L 0.000 claims abstract description 14
- 229940074439 potassium sodium tartrate Drugs 0.000 claims abstract description 14
- 235000011006 sodium potassium tartrate Nutrition 0.000 claims abstract description 14
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 12
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 12
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- 239000008367 deionised water Substances 0.000 claims description 27
- 229910021641 deionized water Inorganic materials 0.000 claims description 27
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 24
- 238000005554 pickling Methods 0.000 claims description 18
- 239000003792 electrolyte Substances 0.000 claims description 15
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 12
- 235000019832 sodium triphosphate Nutrition 0.000 claims description 12
- ZANJCVQHFYUWGP-UHFFFAOYSA-N S(=S)(=O)(O)O.OCCC[Na] Chemical compound S(=S)(=O)(O)O.OCCC[Na] ZANJCVQHFYUWGP-UHFFFAOYSA-N 0.000 claims description 10
- 229940045998 sodium isethionate Drugs 0.000 claims description 10
- LADXKQRVAFSPTR-UHFFFAOYSA-M sodium;2-hydroxyethanesulfonate Chemical compound [Na+].OCCS([O-])(=O)=O LADXKQRVAFSPTR-UHFFFAOYSA-M 0.000 claims description 10
- 238000005406 washing Methods 0.000 claims description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims description 8
- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 claims description 8
- 235000021110 pickles Nutrition 0.000 claims description 6
- FTLYMKDSHNWQKD-UHFFFAOYSA-N (2,4,5-trichlorophenyl)boronic acid Chemical compound OB(O)C1=CC(Cl)=C(Cl)C=C1Cl FTLYMKDSHNWQKD-UHFFFAOYSA-N 0.000 claims description 3
- 229940085605 saccharin sodium Drugs 0.000 claims description 3
- 239000011248 coating agent Substances 0.000 abstract description 41
- 238000000576 coating method Methods 0.000 abstract description 41
- 150000003839 salts Chemical class 0.000 abstract description 2
- 239000008139 complexing agent Substances 0.000 abstract 1
- 238000004140 cleaning Methods 0.000 description 7
- 239000010410 layer Substances 0.000 description 7
- 238000004381 surface treatment Methods 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 229910052708 sodium Inorganic materials 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- ZDVYABSQRRRIOJ-UHFFFAOYSA-N boron;iron Chemical compound [Fe]#B ZDVYABSQRRRIOJ-UHFFFAOYSA-N 0.000 description 1
- 230000003749 cleanliness Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- QEFYFXOXNSNQGX-UHFFFAOYSA-N neodymium atom Chemical compound [Nd] QEFYFXOXNSNQGX-UHFFFAOYSA-N 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- Electroplating Methods And Accessories (AREA)
- Electroplating And Plating Baths Therefor (AREA)
Abstract
本发明公开了一种钕铁硼薄片磁钢产品的电镀镍方法，先后通过预镀镍处理、镀半光镍处理和镀光亮镍处理，在预镀镍处理过程中，采用双脉冲电源，并且双脉冲电源使用较高的电流密度，由此在预镀镍处理后钕铁硼薄片磁钢产品的表面形成密度大、硬度高、孔隙率低且均匀性高的预镀镍镀层，在后续镀半光镍处理过程中，半光镍溶液由硫酸镍、氯化镍、硼酸、酒石酸钾钠、三乙醇胺、硫酸铵、氨水和水按照特定的配比组成，半光镍溶液中酒石酸钾钠作为配位剂，硫酸铵作为导电盐，提高半光镍镀层的均匀性，最后在半光镍镀层上生成均匀性高的光亮镍层；优点是镀镍层由均匀性高的预镀镍层、半光镍层和光亮镍层组成，大大改善钕铁硼薄片磁钢产品镀层分布均匀性。
The invention discloses a nickel electroplating method for NdFeB thin-slice magnetic steel products, which successively undergoes pre-nickel plating treatment, semi-bright nickel plating treatment and bright nickel plating treatment. During the pre-nickel plating treatment process, a double pulse power supply is used, and The dual-pulse power supply uses a higher current density, so that after the pre-nickeling treatment, the surface of the NdFeB thin sheet magnet product forms a pre-plating nickel coating with high density, high hardness, low porosity and high uniformity. During the semi-gloss nickel treatment process, the semi-gloss nickel solution is composed of nickel sulfate, nickel chloride, boric acid, potassium sodium tartrate, triethanolamine, ammonium sulfate, ammonia water and water according to a specific ratio, and the potassium sodium tartrate in the semi-gloss nickel solution is used as As a complexing agent, ammonium sulfate is used as a conductive salt to improve the uniformity of the semi-gloss nickel coating, and finally a bright nickel layer with high uniformity is formed on the semi-gloss nickel coating; Composed of semi-bright nickel layer and bright nickel layer, it greatly improves the uniformity of coating distribution of NdFeB thin sheet magnet products.
Description
技术领域technical field
本发明涉及一种电镀镍方法，尤其是涉及一种钕铁硼薄片磁钢产品的电镀镍方法。The invention relates to a nickel electroplating method, in particular to a nickel electroplating method for neodymium-iron-boron thin-slice magnetic steel products.
背景技术Background technique
钕铁硼永磁材料是一种化学活性强的粉末材料，其特性硬而脆，易被氧化腐蚀，由此采用钕铁硼永磁材料制备而成的钕铁硼磁钢产品的防腐蚀性能较差。目前，钕铁硼磁钢产品采取的最有效的防腐蚀方法就是采用表面处理方法在钕铁硼磁钢产品的表面形成防护层。由于钕铁硼磁钢产品的表面存在磨削加工时产生的恶化层、密度化不完全而产生的空孔和氧化相等，其表面处理工艺通常包括必要的前处理和适当的电镀工艺。电镀镍结晶极其细小，并且具有优良的抛光性能，经抛光的镍镀层可得到镜面般的光泽外表，同时在大气中可长期保持其光泽，因而目前国内外对钕铁硼磁钢产品较多的采用电镀镍的表面处理方法来进行表面保护。但是现有的电镀镍方法在应用于处理具有厚度薄(厚度≤1mm)、倒角角度较小(倒角半径R≤0.2)和尺寸公差带窄(正负公差≤0.010mm)等特点的钕铁硼薄片磁钢产品时，电力线会过多集中在钕铁硼薄片磁钢产品边缘和尖端，常常出现“边缘效应”和“尖端效应”，使该处的镀层较其他部位较厚，导致产品端部尺寸与中心点尺寸厚度差过大，由此造成镀层分布均匀性不良，直接影响到产品整体装配。NdFeB permanent magnet material is a powder material with strong chemical activity. Its characteristics are hard and brittle, and it is easy to be oxidized and corroded. The corrosion resistance of NdFeB magnet products made of NdFeB permanent magnet materials poor. At present, the most effective anti-corrosion method adopted by NdFeB magnet products is to use surface treatment methods to form a protective layer on the surface of NdFeB magnet products. Since the surface of NdFeB magnet products has a deteriorated layer produced during grinding, voids and oxidation caused by incomplete densification, the surface treatment process usually includes necessary pre-treatment and appropriate electroplating process. Electroplated nickel crystals are extremely small and have excellent polishing properties. The polished nickel coating can obtain a mirror-like glossy appearance, and at the same time maintain its luster for a long time in the atmosphere. Therefore, there are currently many NdFeB magnet products at home and abroad. The surface treatment method of electroplating nickel is used for surface protection. However, the existing electroplating nickel method is applied to the treatment of neodymium with the characteristics of thin thickness (thickness ≤ 1mm), small chamfering angle (chamfering radius R ≤ 0.2) and narrow dimensional tolerance band (positive and negative tolerance ≤ 0.010mm). When using iron-boron thin-film magnet products, the power lines will be too concentrated on the edge and tip of the NdFeB thin-film magnet product, and "edge effect" and "tip effect" often appear, making the coating at this place thicker than other parts, resulting in product failure. The thickness difference between the end size and the center point size is too large, which will cause poor uniformity of coating distribution and directly affect the overall assembly of the product.
鉴此，设计一种可以改善钕铁硼薄片磁钢产品镀层分布均匀性的钕铁硼薄片磁钢产品的电镀镍方法对钕铁硼薄片磁钢产品的表面处理工艺的发展具有重要意义。In view of this, it is of great significance to design a nickel plating method for NdFeB thin sheet magnet products that can improve the coating distribution uniformity of NdFeB thin sheet magnet products for the development of the surface treatment process of NdFeB thin sheet magnet products.
发明内容Contents of the invention
本发明所要解决的技术问题是提供一种可以改善钕铁硼薄片磁钢产品镀层分布均匀性的钕铁硼薄片磁钢产品的电镀镍方法。The technical problem to be solved by the present invention is to provide a nickel electroplating method for NdFeB thin sheet magnetic steel products that can improve the uniformity of coating distribution of the NdFeB thin sheet magnetic steel products.
本发明解决上述技术问题所采用的技术方案为：一种钕铁硼薄片磁钢产品的电镀镍方法，包括以下步骤：The technical scheme adopted by the present invention to solve the above-mentioned technical problems is: a method for electroplating nickel of neodymium-iron-boron thin-sheet magnetic steel products, comprising the following steps:
①对钕铁硼薄片磁钢产品进行前处理；① Pretreatment of NdFeB thin sheet magnet products;
②对钕铁硼薄片磁钢产品进行预镀镍处理：预镀镍溶液由硫酸镍、硼酸、羟乙基磺酸钠、羟丙基硫代硫酸钠和水组成，硫酸镍的质量体积浓度为220～300克/升，硼酸的质量体积浓度为30～50克/升，羟乙基磺酸钠的质量体积浓度为10～25毫克/升，羟丙基硫代硫酸钠的质量体积浓度为2～8毫克/升，预镀镍处理时间为3500～6500秒，预镀镍处理过程中采用双脉冲电源，其正向电流密度为0.2～0.8安培/平方分米，反向电流密度为0.1～0.3安培/平方分米，正向导通时间为10～20秒，反向导通时间为5～10秒，正向频率为1～1.5kHz，反向频率为0.1～0.5kHz，正向占空比为50％～70％，反向占空比为10％～30％，预镀镍溶液的温度为40～60℃，PH值为3.5～4.8；② Pre-nickel-plating treatment of NdFeB thin-sheet magnetic steel products: the pre-nickel plating solution is composed of nickel sulfate, boric acid, sodium isethionate, hydroxypropyl sodium thiosulfate and water, and the mass volume concentration of nickel sulfate is 220～300 g/L, the mass volume concentration of boric acid is 30～50 g/L, the mass volume concentration of sodium isethionate is 10～25 mg/L, the mass volume concentration of hydroxypropyl sodium thiosulfate is 2-8 mg/L, the pre-nickeling treatment time is 3500-6500 seconds, the double-pulse power supply is used in the pre-nickeling process, the forward current density is 0.2-0.8 ampere/square decimeter, and the reverse current density is 0.1 ～0.3 ampere/square decimeter, forward conduction time is 10～20 seconds, reverse conduction time is 5～10 seconds, forward frequency is 1～1.5kHz, reverse frequency is 0.1～0.5kHz, forward duty The ratio is 50%~70%, the reverse duty ratio is 10%~30%, the temperature of the pre-nickel plating solution is 40~60°C, and the pH value is 3.5~4.8;
③采用去离子水对预镀镍处理过的钕铁硼薄片磁钢产品进行多次清洗，将预镀镍处理过的钕铁硼薄片磁钢产品清洗干净；③Using deionized water to clean the pre-nickel-plated NdFeB thin-sheet magnet products several times, and clean the pre-nickel-plated NdFeB thin-sheet magnet products;
④对钕铁硼薄片磁钢产品进行镀半光镍处理：半光镍溶液由硫酸镍、氯化镍、硼酸、酒石酸钾钠、三乙醇胺、硫酸铵、氨水和水组成，硫酸镍的质量体积浓度为100～200克/升，氯化镍的质量体积浓度为20～40克/升，硼酸的质量体积浓度为20～40克/升，酒石酸钾钠质量体积浓度为40～70克/升，三乙醇胺质量体积浓度为20～60克/升，硫酸铵质量体积浓度为10～50克/升，氨水体积百分比浓度为20～60毫升/升，镀半光镍处理时间为3500～5500秒，镀半光镍处理过程中采用高频直流电源，其电流密度为0.2～0.8安培/平方分米，温度为40～60℃，PH值为4.8～6.5；④ Plating semi-bright nickel on NdFeB thin-sheet magnetic steel products: semi-bright nickel solution consists of nickel sulfate, nickel chloride, boric acid, potassium sodium tartrate, triethanolamine, ammonium sulfate, ammonia water and water, the mass volume of nickel sulfate The concentration is 100-200 g/L, the mass volume concentration of nickel chloride is 20-40 g/L, the mass volume concentration of boric acid is 20-40 g/L, and the mass volume concentration of potassium sodium tartrate is 40-70 g/L , the mass volume concentration of triethanolamine is 20-60 g/l, the mass volume concentration of ammonium sulfate is 10-50 g/l, the volume percentage concentration of ammonia water is 20-60 ml/l, and the semi-gloss nickel plating treatment time is 3500-5500 seconds , High-frequency DC power supply is used in the process of semi-gloss nickel plating, the current density is 0.2-0.8 ampere/square decimeter, the temperature is 40-60 ℃, and the pH value is 4.8-6.5;
⑤采用去离子水对镀半光镍处理过的钕铁硼薄片磁钢产品进行多次清洗，将镀半光镍处理过的钕铁硼薄片磁钢产品清洗干净；⑤Using deionized water to clean the NdFeB thin-sheet magnet products treated with semi-bright nickel for several times, and clean the NdFeB thin-sheet magnet products treated with semi-bright nickel;
⑥对钕铁硼薄片磁钢产品进行镀光亮镍处理：光亮镍溶液由硫酸镍、氯化镍、硼酸、糖精钠和水组成，硫酸镍的质量体积浓度为200～300克/升，氯化镍的质量体积浓度为30～60克/升，硼酸的质量体积浓度为30～60克/升，糖精钠的质量体积浓度为5～20毫克/升，镀光亮镍处理时间为2500～4000秒，镀光亮镍处理过程中采用高频直流电源，其电流密度为0.1～0.8安培/平方分米，光亮镍溶液的温度为40～60℃，PH值为3.5～4.8；⑥ Perform bright nickel plating treatment on NdFeB thin sheet magnetic steel products: bright nickel solution is composed of nickel sulfate, nickel chloride, boric acid, sodium saccharin and water. The mass volume concentration of nickel is 30-60 g/L, the mass volume concentration of boric acid is 30-60 g/L, the mass volume concentration of saccharin sodium is 5-20 mg/L, and the bright nickel plating treatment time is 2500-4000 seconds , High-frequency DC power supply is used in the process of bright nickel plating, the current density is 0.1-0.8 ampere/square decimeter, the temperature of bright nickel solution is 40-60 ℃, and the pH value is 3.5-4.8;
⑦采用去离子水对镀光亮镍处理过的钕铁硼薄片磁钢产品进行多次清洗，将镀光亮镍处理过的钕铁硼薄片磁钢产品清洗干净后烘干。⑦ Use deionized water to clean the bright nickel-plated NdFeB thin-slice magnet products several times, clean and dry the bright nickel-plated NdFeB thin-slice magnet products.
所述的步骤①中前处理工艺包括以下步骤：Described step 1. pretreatment process comprises the following steps:
①-1酸洗：采用稀硝酸溶液作为酸洗液对钕铁硼薄片磁钢产品进行酸洗；①-1 Pickling: Use dilute nitric acid solution as the pickling solution to pickle the NdFeB thin sheet magnet products;
①-2水洗：采用去离子水对酸洗后的钕铁硼薄片磁钢产品进行多次清洗，将钕铁硼薄片磁钢产品清洗干净；①-2 Washing: Use deionized water to wash the pickled NdFeB thin sheet magnet products several times, and clean the NdFeB thin sheet magnet products;
①-3将水洗后的钕铁硼薄片磁钢产品放入电解槽中进行电解处理，电解处理时间为250～400秒，电解液由氢氧化钠、碳酸钠、三聚磷酸钠和水组成，氢氧化钠的质量体积浓度为30～60克/升，碳酸钠的质量体积浓度为20～40克/升，三聚磷酸钠的质量体积浓度为20～40克/升，电解处理过程中电流密度为0.2～0.8安培/平方分米，电解液温度为30～60℃；①-3 Put the washed NdFeB thin sheet magnetic steel products into the electrolytic tank for electrolytic treatment. The electrolytic treatment time is 250-400 seconds. The electrolyte is composed of sodium hydroxide, sodium carbonate, sodium tripolyphosphate and water. The mass volume concentration of sodium hydroxide is 30-60 g/L, the mass volume concentration of sodium carbonate is 20-40 g/L, and the mass volume concentration of sodium tripolyphosphate is 20-40 g/L. The density is 0.2-0.8 ampere/square decimeter, and the electrolyte temperature is 30-60°C;
①-4水洗：采用去离子水对电解后的钕铁硼薄片磁钢产品进行多次清洗，将钕铁硼薄片磁钢产品清洗干净。①-4Water washing: use deionized water to wash the electrolyzed NdFeB thin sheet magnet products several times, and clean the NdFeB thin sheet magnet products.
与现有技术相比，本发明的优点在于在预镀镍处理过程中，采用双脉冲电源，并且双脉冲电源使用较高的电流密度，使预镀镍处理过程中晶核的形成速率远远大于原有晶体的生长速率，可在钕铁硼薄片磁钢产品形成结晶细致的预镀镍镀层，同时，在预镀镍处理过程中，脉冲电源的脉冲按照周期交替开启和关断，在脉冲关断期内，阴极区域预镀镍溶液中导电离子的质量浓度会得到不同程度的回升，由此预镀镍溶液的电阻率会减小，预镀镍溶液中导电离子的分散均匀性得到改善，提高预镀镍镀层的均匀性，由此预镀镍处理后钕铁硼薄片磁钢产品的表面形成密度大、硬度高、孔隙率低且均匀性高的预镀镍镀层，在后续镀半光镍处理过程中，半光镍溶液由硫酸镍、氯化镍、硼酸、酒石酸钾钠、三乙醇胺、硫酸铵、氨水和水按照特定的配比组成，半光镍溶液中酒石酸钾钠作为配位剂，硫酸铵作为导电盐，由此可增加镀半光镍处理过程中半光镍溶液阴极的极化度和提高半光镍溶液的导电性，减小半光镍溶液的电阻率，提高半光镍溶液中导电离子的分散能力，提高半光镍镀层的均匀性，最后采用由硫酸镍、氯化镍、硼酸、糖精钠和水按照特定配比组成的光亮镍溶液进行镀光亮镍处理，在半光镍镀层上生成均匀性高的光亮镍层，由此最终的镀镍层由均匀性高的预镀镍层、半光镍层和光亮镍层组成，大大改善钕铁硼薄片磁钢产品镀层分布均匀性；Compared with the prior art, the advantage of the present invention is that in the pre-nickeling process, a double-pulse power supply is used, and the double-pulse power supply uses a higher current density, so that the formation rate of crystal nuclei in the pre-nickeling process is much larger. Due to the growth rate of the original crystal, a fine crystalline pre-nickel coating can be formed on the NdFeB thin sheet magnet products. During the shutdown period, the mass concentration of conductive ions in the pre-nickel solution in the cathode area will be recovered to varying degrees, so the resistivity of the pre-nickel solution will decrease, and the dispersion uniformity of conductive ions in the pre-nickel solution will be improved. , improve the uniformity of the pre-plating nickel coating, so that the surface of the NdFeB thin sheet magnetic steel product after the pre-nickeling treatment forms a pre-plating nickel coating with high density, high hardness, low porosity and high uniformity. During the light nickel treatment process, the semi-bright nickel solution is composed of nickel sulfate, nickel chloride, boric acid, potassium sodium tartrate, triethanolamine, ammonium sulfate, ammonia water and water according to a specific ratio, and the semi-bright nickel solution is composed of potassium sodium tartrate As a conductive salt, ammonium sulfate can increase the polarizability of the cathode of the semi-gloss nickel solution in the semi-gloss nickel plating process and improve the conductivity of the semi-gloss nickel solution, reduce the resistivity of the semi-gloss nickel solution, and improve the conductivity of the semi-gloss nickel solution. The dispersing ability of conductive ions in the semi-gloss nickel solution improves the uniformity of the semi-gloss nickel coating. Finally, the bright nickel solution composed of nickel sulfate, nickel chloride, boric acid, sodium saccharin and water according to a specific ratio is used for bright nickel plating. , A bright nickel layer with high uniformity is formed on the semi-bright nickel layer, and the final nickel layer is composed of a pre-plated nickel layer, a semi-bright nickel layer and a bright nickel layer with high uniformity, which greatly improves the magnetic properties of NdFeB thin sheets. Uniformity of coating distribution of steel products;
当步骤①中前处理工艺包括以下步骤：When step 1. the pretreatment process comprises the following steps:
①-1酸洗：采用稀硝酸溶液作为酸洗液对钕铁硼薄片磁钢产品进行酸洗；①-1 Pickling: Use dilute nitric acid solution as the pickling solution to pickle the NdFeB thin sheet magnet products;
①-2水洗：采用去离子水对酸洗后的钕铁硼薄片磁钢产品进行多次清洗，将钕铁硼薄片磁钢产品清洗干净；①-2 Washing: Use deionized water to wash the pickled NdFeB thin sheet magnet products several times, and clean the NdFeB thin sheet magnet products;
①-3将水洗后的钕铁硼薄片磁钢产品放入电解槽中进行电解处理，电解处理时间为250～400秒，电解液由氢氧化钠、碳酸钠、三聚磷酸钠和水组成，氢氧化钠的质量体积浓度为30～60克/升，碳酸钠的质量体积浓度为20～40克/升，三聚磷酸钠的质量体积浓度为20～40克/升，电解处理过程中电流密度为0.2～0.8安培/平方分米，电解液温度为30～60℃；①-3 Put the washed NdFeB thin sheet magnetic steel products into the electrolytic tank for electrolytic treatment. The electrolytic treatment time is 250-400 seconds. The electrolyte is composed of sodium hydroxide, sodium carbonate, sodium tripolyphosphate and water. The mass volume concentration of sodium hydroxide is 30-60 g/L, the mass volume concentration of sodium carbonate is 20-40 g/L, and the mass volume concentration of sodium tripolyphosphate is 20-40 g/L. The density is 0.2-0.8 ampere/square decimeter, and the electrolyte temperature is 30-60°C;
①-4水洗：采用去离子水对电解后的钕铁硼薄片磁钢产品进行多次清洗，将钕铁硼薄片磁钢产品清洗干净时，具有以下优点：首先在酸洗中采用稀硝酸溶液作为酸洗液，稀硝酸不会对钕铁硼磁体结构造成损害，减少酸洗对磁性能的影响，然后采用水洗、电解和再次水洗的工艺对钕铁硼磁体进行处理，可以去除钕铁硼磁体在前道工序中附着的油污和表面氧化物等，保证钕铁硼磁体表面在入电镀槽前处于活性状态，具有较好的清洁度和磁性能。①-4Washing: Use deionized water to clean the electrolyzed NdFeB flake magnet products several times. When cleaning the NdFeB flake magnet products, it has the following advantages: First, dilute nitric acid solution is used in pickling As a pickling solution, dilute nitric acid will not damage the structure of NdFeB magnets and reduce the impact of pickling on the magnetic properties. Then the NdFeB magnets will be treated with water washing, electrolysis and water washing again to remove NdFeB magnets. The oil stains and surface oxides attached to the magnet in the previous process ensure that the surface of the NdFeB magnet is in an active state before entering the electroplating tank, and has good cleanliness and magnetic properties.
附图说明Description of drawings
图1为本发明的实施例中钕铁硼薄片磁钢产品的结构示意图。Fig. 1 is a schematic structural view of an NdFeB thin sheet magnet product in an embodiment of the present invention.
具体实施方式detailed description
以下结合附图实施例对本发明作进一步详细描述。The present invention will be further described in detail below in conjunction with the accompanying drawings and embodiments.
实施例一：一种钕铁硼薄片磁钢产品的电镀镍方法，包括以下步骤：Embodiment one: a kind of electroplating nickel method of NdFeB sheet magnetic steel product, comprises the following steps:
①钕铁硼薄片磁钢产品进行前处理；① Pre-treatment of NdFeB thin sheet magnet products;
②对钕铁硼薄片磁钢产品进行预镀镍处理：预镀镍溶液由硫酸镍、硼酸、羟乙基磺酸钠、羟丙基硫代硫酸钠和水组成，硫酸镍的质量体积浓度为220克/升，硼酸的质量体积浓度为30克/升，羟乙基磺酸钠的质量体积浓度为10毫克/升，羟丙基硫代硫酸钠的质量体积浓度为2毫克/升，预镀镍处理时间为3500秒，预镀镍处理过程中采用双脉冲电源，其正向电流密度为0.2安培/平方分米，反向电流密度为0.1安培/平方分米，正向导通时间为10秒，反向导通时间为5秒，正向频率为1kHz，反向频率为0.1kHz，正向占空比为50％，反向占空比为10％，预镀镍溶液的温度为40℃，PH值为3.5；② Pre-nickel-plating treatment of NdFeB thin-sheet magnetic steel products: the pre-nickel plating solution is composed of nickel sulfate, boric acid, sodium isethionate, hydroxypropyl sodium thiosulfate and water, and the mass volume concentration of nickel sulfate is 220 grams per liter, the mass volume concentration of boric acid is 30 grams per liter, the mass volume concentration of sodium isethionate is 10 mg/liter, and the mass volume concentration of hydroxypropyl sodium thiosulfate is 2 mg/liter. Nickel plating treatment time is 3500 seconds, double pulse power supply is used in the process of pre-nickel plating, the forward current density is 0.2 ampere/dm2, the reverse current density is 0.1 ampere/dm2, and the forward conduction time is 10 seconds, the reverse conduction time is 5 seconds, the forward frequency is 1kHz, the reverse frequency is 0.1kHz, the forward duty cycle is 50%, the reverse duty cycle is 10%, the temperature of the pre-nickel solution is 40℃ , the pH value is 3.5;
③采用去离子水对预镀镍处理过的钕铁硼薄片磁钢产品进行多次清洗，将预镀镍处理过的钕铁硼薄片磁钢产品清洗干净；清洗次数根据现有常规的电镀工艺选择，将表面残留的镀液清洗干净即可；③ Use deionized water to clean the pre-nickel-plated NdFeB thin-slice magnet products several times, and clean the pre-nickel-plated NdFeB thin-slice magnet products; the number of cleanings is based on the existing conventional electroplating process Select, just clean the residual plating solution on the surface;
④对钕铁硼薄片磁钢产品进行镀半光镍处理：半光镍溶液由硫酸镍、氯化镍、硼酸、酒石酸钾钠、三乙醇胺、硫酸铵、氨水和水组成，硫酸镍的质量体积浓度为100克/升，氯化镍的质量体积浓度为20克/升，硼酸的质量体积浓度为20克/升，酒石酸钾钠质量体积浓度为40克/升，三乙醇胺质量体积浓度为20克/升，硫酸铵质量体积浓度为10克/升，氨水体积百分比浓度为20毫升/升，镀半光镍处理时间为3500秒，镀半光镍处理过程中采用高频直流电源，其电流密度为0.2安培/平方分米，温度为40℃，PH值为4.8；④ Plating semi-bright nickel on NdFeB thin-sheet magnetic steel products: semi-bright nickel solution consists of nickel sulfate, nickel chloride, boric acid, potassium sodium tartrate, triethanolamine, ammonium sulfate, ammonia water and water, the mass volume of nickel sulfate Concentration is 100 grams/liter, and the mass volume concentration of nickel chloride is 20 grams/liter, and the mass volume concentration of boric acid is 20 grams/liter, and potassium sodium tartrate mass volume concentration is 40 grams/liter, and triethanolamine mass volume concentration is 20 gram/liter, the mass volume concentration of ammonium sulfate is 10 grams/liter, the volume percentage concentration of ammonia water is 20 milliliters/liter, the treatment time of semi-gloss nickel plating is 3500 seconds, and a high-frequency direct current power supply is adopted in the process of semi-gloss nickel plating, and its current The density is 0.2 ampere/square decimeter, the temperature is 40°C, and the pH value is 4.8;
⑤采用去离子水对镀半光镍处理过的钕铁硼薄片磁钢产品进行多次清洗，将镀半光镍处理过的钕铁硼薄片磁钢产品清洗干净；清洗次数根据现有常规的电镀工艺选择，将表面残留的镀液清洗干净即可；⑤ Use deionized water to clean the semi-bright nickel-plated NdFeB thin-sheet magnet products several times, and clean the semi-bright nickel-plated NdFeB thin-sheet magnet products; the number of cleanings is based on the existing conventional Electroplating process selection, just clean the remaining plating solution on the surface;
⑥对钕铁硼薄片磁钢产品进行镀光亮镍处理：光亮镍溶液由硫酸镍、氯化镍、硼酸、糖精钠和水组成，硫酸镍的质量体积浓度为200克/升，氯化镍的质量体积浓度为30克/升，硼酸的质量体积浓度为30克/升，糖精钠的质量体积浓度为5毫克/升，镀光亮镍处理时间为2500秒，镀光亮镍处理过程中采用高频直流电源，其电流密度为0.1安培/平方分米，光亮镍溶液的温度为40℃，PH值为3.5；⑥ Perform bright nickel plating treatment on NdFeB thin sheet magnetic steel products: bright nickel solution is composed of nickel sulfate, nickel chloride, boric acid, sodium saccharin and water, the mass volume concentration of nickel sulfate is 200 g/L, and the concentration of nickel chloride The mass volume concentration is 30 g/l, the mass volume concentration of boric acid is 30 g/l, the mass volume concentration of sodium saccharin is 5 mg/l, the bright nickel plating treatment time is 2500 seconds, and high frequency is used in the bright nickel plating process DC power supply, its current density is 0.1 ampere/square decimeter, the temperature of bright nickel solution is 40 ℃, and the pH value is 3.5;
⑦采用去离子水对镀光亮镍处理过的钕铁硼薄片磁钢产品进行多次清洗，将镀光亮镍处理过的钕铁硼薄片磁钢产品清洗干净后烘干。⑦ Use deionized water to clean the bright nickel-plated NdFeB thin-slice magnet products several times, clean and dry the bright nickel-plated NdFeB thin-slice magnet products.
本实施例中，步骤①中前处理工艺包括以下步骤：In the present embodiment, the pretreatment process in step 1. includes the following steps:
①-1酸洗：采用稀硝酸溶液作为酸洗液对钕铁硼薄片磁钢产品进行酸洗；①-1 Pickling: Use dilute nitric acid solution as the pickling solution to pickle the NdFeB thin sheet magnet products;
①-2水洗：采用去离子水对酸洗后的钕铁硼薄片磁钢产品进行多次清洗，将表面残留的酸洗液清洗干净；①-2 Washing: Use deionized water to wash the pickled NdFeB thin sheet magnet products several times, and clean the residual pickling solution on the surface;
①-3将水洗后的钕铁硼薄片磁钢产品放入电解槽中进行电解处理，电解处理时间为250秒，电解液由氢氧化钠、碳酸钠、三聚磷酸钠和水组成，氢氧化钠的质量体积浓度为30克/升，碳酸钠的质量体积浓度为20克/升，三聚磷酸钠的质量体积浓度为20克/升，电解处理过程中电流密度为0.2安培/平方分米，电解液温度为30℃；①-3 Put the washed NdFeB thin sheet magnetic steel products into the electrolytic tank for electrolytic treatment. The electrolytic treatment time is 250 seconds. The electrolyte is composed of sodium hydroxide, sodium carbonate, sodium tripolyphosphate and water. The mass volume concentration of sodium is 30 grams/liter, the mass volume concentration of sodium carbonate is 20 grams/liter, the mass volume concentration of sodium tripolyphosphate is 20 grams/liter, and the current density during electrolytic treatment is 0.2 ampere/square decimeter , the electrolyte temperature is 30°C;
①-4水洗：采用去离子水对电解后的钕铁硼薄片磁钢产品进行多次清洗，将表面残留的电解液清洗干净。①-4Washing: Use deionized water to wash the electrolyzed NdFeB thin sheet magnet products several times to clean the residual electrolyte on the surface.
采用本实施例的方法对厚度为0.900±0.010毫米、端面积为2.88平方厘米、周长为7.95厘米、轮廓度为0.28、倒角值为0.25的钕铁硼薄片磁钢产品进行处理，薄片磁钢产品具体结构如图1所示。将上述钕铁硼薄片磁钢产品分成A组、B组和C组三组，分别采用本实施例的方法进行电镀镍处理，相应得到A组、B组和C组三组电镀镍后的产品。对A组、B组和C组三组电镀镍后的产品的镀层分布均匀性进行检测，其中镀层分布均匀性为产品尖端部与产品中心部镀层厚度的比值，比值越小，镀层分布均匀性越好。A组、B组和C组三组产品镀层分布均匀性：钕铁硼薄片磁钢产品的B点(即产品尖端部)镀层厚度与A点(即产品中心部)镀层厚度的比值如下表1所示。Adopt the method of this embodiment to process the neodymium-iron-boron thin sheet magnetic steel products with a thickness of 0.900 ± 0.010 mm, an end area of 2.88 square centimeters, a circumference of 7.95 cm, a contour of 0.28, and a chamfer value of 0.25. The specific structure of steel products is shown in Figure 1. Divide the above-mentioned NdFeB thin sheet magnetic steel products into three groups of A group, B group and C group, respectively adopt the method of this embodiment to carry out nickel plating treatment, and obtain the products of A group, B group and C group three groups after electroplating nickel correspondingly . The coating distribution uniformity of the nickel-plated products in Group A, Group B and Group C is tested. The coating distribution uniformity is the ratio of the thickness of the coating at the tip of the product to the center of the product. The smaller the ratio, the more uniform the coating distribution. the better. The uniformity of the coating distribution of the three groups of products in Group A, Group B and Group C: the ratio of the thickness of the coating at point B (that is, the tip of the product) of the NdFeB sheet magnet product to the thickness of the coating at point A (that is, the center of the product) is shown in Table 1 shown.
表1Table 1
分析表1数据可知，采用本实施例的方法处理的钕铁硼薄片磁钢产品的镀层分布均匀性优良。From the analysis of the data in Table 1, it can be known that the coating distribution uniformity of the NdFeB thin sheet magnet products processed by the method of this embodiment is excellent.
实施例二：一种钕铁硼薄片磁钢产品的电镀镍方法，包括以下步骤：Embodiment two: a kind of electroplating nickel method of NdFeB sheet magnetic steel product, comprises the following steps:
①对钕铁硼薄片磁钢产品进行前处理；① Pretreatment of NdFeB thin sheet magnet products;
②对钕铁硼薄片磁钢产品进行预镀镍处理：预镀镍溶液由硫酸镍、硼酸、羟乙基磺酸钠、羟丙基硫代硫酸钠和水组成，硫酸镍的质量体积浓度为300克/升，硼酸的质量体积浓度为50克/升，羟乙基磺酸钠的质量体积浓度为25毫克/升，羟丙基硫代硫酸钠的质量体积浓度为8毫克/升，预镀镍处理时间为6500秒，预镀镍处理过程中采用双脉冲电源，其正向电流密度为0.8安培/平方分米，反向电流密度为0.3安培/平方分米，正向导通时间为20秒，反向导通时间为10秒，正向频率为1.5kHz，反向频率为0.5kHz，正向占空比为70％，反向占空比为30％，预镀镍溶液的温度为60℃，PH值为4.8；② Pre-nickel-plating treatment of NdFeB thin-sheet magnetic steel products: the pre-nickel plating solution is composed of nickel sulfate, boric acid, sodium isethionate, hydroxypropyl sodium thiosulfate and water, and the mass volume concentration of nickel sulfate is 300 grams/liter, the mass volume concentration of boric acid is 50 grams/liter, the mass volume concentration of sodium isethionate is 25 mg/liter, and the mass volume concentration of hydroxypropyl sodium thiosulfate is 8 mg/liter. The nickel plating treatment time is 6500 seconds, and the double pulse power supply is used in the pre-nickel plating process. The forward current density is 0.8 ampere/square decimeter, the reverse current density is 0.3 ampere/square decimeter, and the forward conduction time is 20 seconds, the reverse conduction time is 10 seconds, the forward frequency is 1.5kHz, the reverse frequency is 0.5kHz, the forward duty cycle is 70%, the reverse duty cycle is 30%, the temperature of the pre-nickel solution is 60 °C, pH value is 4.8;
③采用去离子水对预镀镍处理过的钕铁硼薄片磁钢产品进行多次清洗，将预镀镍处理过的钕铁硼薄片磁钢产品清洗干净；清洗次数根据现有常规的电镀工艺选择，将表面残留的镀液清洗干净即可；③ Use deionized water to clean the pre-nickel-plated NdFeB thin-slice magnet products several times, and clean the pre-nickel-plated NdFeB thin-slice magnet products; the number of cleanings is based on the existing conventional electroplating process Select, just clean the residual plating solution on the surface;
④对钕铁硼薄片磁钢产品进行镀半光镍处理：半光镍溶液由硫酸镍、氯化镍、硼酸、酒石酸钾钠、三乙醇胺、硫酸铵、氨水和水组成，硫酸镍的质量体积浓度为200克/升，氯化镍的质量体积浓度为40克/升，硼酸的质量体积浓度为40克/升，酒石酸钾钠质量体积浓度为70克/升，三乙醇胺质量体积浓度为60克/升，硫酸铵质量体积浓度为50克/升，氨水体积百分比浓度为60毫升/升，镀半光镍处理时间为5500秒，镀半光镍处理过程中采用高频直流电源，其电流密度为0.8安培/平方分米，温度为60℃，PH值为6.5；④ Plating semi-bright nickel on NdFeB thin-sheet magnetic steel products: semi-bright nickel solution consists of nickel sulfate, nickel chloride, boric acid, potassium sodium tartrate, triethanolamine, ammonium sulfate, ammonia water and water, the mass volume of nickel sulfate Concentration is 200 grams/liter, and the mass volume concentration of nickel chloride is 40 grams/liter, and the mass volume concentration of boric acid is 40 grams/liter, and potassium sodium tartrate mass volume concentration is 70 grams/liter, and triethanolamine mass volume concentration is 60 gram/liter, the mass volume concentration of ammonium sulfate is 50 grams/liter, the volume percentage concentration of ammonia water is 60 milliliters/liter, the treatment time of semi-gloss nickel plating is 5500 seconds, and a high-frequency direct current power supply is adopted in the process of semi-gloss nickel plating, and its current The density is 0.8 ampere/square decimeter, the temperature is 60°C, and the pH value is 6.5;
⑤采用去离子水对镀半光镍处理过的钕铁硼薄片磁钢产品进行多次清洗，将镀半光镍处理过的钕铁硼薄片磁钢产品清洗干净；清洗次数根据现有常规的电镀工艺选择，将表面残留的镀液清洗干净即可；⑤ Use deionized water to clean the semi-bright nickel-plated NdFeB thin-sheet magnet products several times, and clean the semi-bright nickel-plated NdFeB thin-sheet magnet products; the number of cleanings is based on the existing conventional Electroplating process selection, just clean the remaining plating solution on the surface;
⑥对钕铁硼薄片磁钢产品进行镀光亮镍处理：光亮镍溶液由硫酸镍、氯化镍、硼酸、糖精钠和水组成，硫酸镍的质量体积浓度为300克/升，氯化镍的质量体积浓度为60克/升，硼酸的质量体积浓度为60克/升，糖精钠的质量体积浓度为20毫克/升，镀光亮镍处理时间为4000秒，镀光亮镍处理过程中采用高频直流电源，其电流密度为0.8安培/平方分米，光亮镍溶液的温度为60℃，PH值为4.8；⑥ Perform bright nickel plating treatment on NdFeB thin sheet magnetic steel products: bright nickel solution is composed of nickel sulfate, nickel chloride, boric acid, sodium saccharin and water, the mass volume concentration of nickel sulfate is 300 g/L, and the concentration of nickel chloride The mass volume concentration is 60 g/l, the mass volume concentration of boric acid is 60 g/l, the mass volume concentration of sodium saccharin is 20 mg/l, the bright nickel plating treatment time is 4000 seconds, and high frequency is used in the bright nickel plating process DC power supply, its current density is 0.8 ampere/square decimeter, the temperature of bright nickel solution is 60 ℃, and the pH value is 4.8;
⑦采用去离子水对镀光亮镍处理过的钕铁硼薄片磁钢产品进行多次清洗，将镀光亮镍处理过的钕铁硼薄片磁钢产品清洗干净后烘干。⑦ Use deionized water to clean the bright nickel-plated NdFeB thin-slice magnet products several times, clean and dry the bright nickel-plated NdFeB thin-slice magnet products.
本实施例中，步骤①中前处理工艺包括以下步骤：In the present embodiment, the pretreatment process in step 1. includes the following steps:
①-1酸洗：采用稀硝酸溶液作为酸洗液对钕铁硼薄片磁钢产品进行酸洗；①-1 Pickling: Use dilute nitric acid solution as the pickling solution to pickle the NdFeB thin sheet magnet products;
①-2水洗：采用去离子水对酸洗后的钕铁硼薄片磁钢产品进行多次清洗，将表面残留的酸洗液清洗干净；①-2 Washing: Use deionized water to wash the pickled NdFeB thin sheet magnet products several times, and clean the residual pickling solution on the surface;
①-3将水洗后的钕铁硼薄片磁钢产品放入电解槽中进行电解处理，电解处理时间为400秒，电解液由氢氧化钠、碳酸钠、三聚磷酸钠和水组成，氢氧化钠的质量体积浓度为60克/升，碳酸钠的质量体积浓度为40克/升，三聚磷酸钠的质量体积浓度为40克/升，电解处理过程中电流密度为0.8安培/平方分米，电解液温度为60℃；①-3 Put the washed NdFeB thin sheet magnetic steel products into the electrolytic tank for electrolytic treatment. The electrolytic treatment time is 400 seconds. The electrolyte is composed of sodium hydroxide, sodium carbonate, sodium tripolyphosphate and water. The mass volume concentration of sodium is 60 grams/liter, the mass volume concentration of sodium carbonate is 40 grams/liter, the mass volume concentration of sodium tripolyphosphate is 40 grams/liter, and the current density during electrolytic treatment is 0.8 ampere/square decimeter , the electrolyte temperature is 60°C;
①-4水洗：用去离子水对电解后的钕铁硼薄片磁钢产品进行多次清洗，将表面残留的电解液清洗干净。①-4Washing: Use deionized water to wash the electrolyzed NdFeB thin sheet magnet products several times to clean the residual electrolyte on the surface.
采用本实施例的方法对厚度为0.900±0.010毫米、端面积为2.88平方厘米、周长为7.95厘米、轮廓度为0.28、倒角值为0.25的钕铁硼薄片磁钢产品进行处理，薄片磁钢产品具体结构如图1所示。将上述钕铁硼薄片磁钢产品分成A组、B组和C组三组，分别采用本实施例的方法进行电镀镍处理，相应得到A组、B组和C组三组电镀镍后的产品。对A组、B组和C组三组电镀镍后的产品的镀层分布均匀性进行检测，其中镀层分布均匀性为产品尖端部与产品中心部镀层厚度的比值，比值越小，镀层分布均匀性越好。A组、B组和C组三组产品镀层分布均匀性：钕铁硼薄片磁钢产品的B点(即产品尖端部)镀层厚度与A点(即产品中心部)镀层厚度的比值如下表2所示。Adopt the method of this embodiment to process the neodymium-iron-boron thin sheet magnetic steel products with a thickness of 0.900 ± 0.010 mm, an end area of 2.88 square centimeters, a circumference of 7.95 cm, a contour of 0.28, and a chamfer value of 0.25. The specific structure of steel products is shown in Figure 1. Divide the above-mentioned NdFeB thin sheet magnetic steel products into three groups of A group, B group and C group, respectively adopt the method of this embodiment to carry out nickel plating treatment, and obtain the products of A group, B group and C group three groups after electroplating nickel correspondingly . The coating distribution uniformity of the nickel-plated products in Group A, Group B and Group C is tested. The coating distribution uniformity is the ratio of the thickness of the coating at the tip of the product to the center of the product. The smaller the ratio, the more uniform the coating distribution. the better. The uniformity of the coating distribution of the three groups of products in Group A, Group B and Group C: the ratio of the thickness of the coating at point B (that is, the tip of the product) of the NdFeB sheet magnet product to the thickness of the coating at point A (that is, the center of the product) is shown in Table 2 shown.
表2Table 2
分析表2数据可知，采用本实施例的方法处理的钕铁硼薄片磁钢产品的镀层分布均匀性优良。From the analysis of the data in Table 2, it can be known that the NdFeB flake magnet products processed by the method of this embodiment have excellent coating distribution uniformity.
实施例三：一种钕铁硼薄片磁钢产品的电镀镍方法，包括以下步骤：Embodiment three: a kind of electroplating nickel method of neodymium-iron-boron sheet magnetic steel product, comprises the following steps:
①对钕铁硼薄片磁钢产品进行前处理；① Pretreatment of NdFeB thin sheet magnet products;
②对钕铁硼薄片磁钢产品进行预镀镍处理：预镀镍溶液由硫酸镍、硼酸、羟乙基磺酸钠、羟丙基硫代硫酸钠和水组成，硫酸镍的质量体积浓度为250克/升，硼酸的质量体积浓度为40克/升，羟乙基磺酸钠的质量体积浓度为20毫克/升，羟丙基硫代硫酸钠的质量体积浓度为5毫克/升，预镀镍处理时间为5000秒，预镀镍处理过程中采用双脉冲电源，其正向电流密度为0.6安培/平方分米，反向电流密度为0.2安培/平方分米，正向导通时间为15秒，反向导通时间为8秒，正向频率为1.2kHz，反向频率为0.3kHz，正向占空比为60％，反向占空比为20％，预镀镍溶液的温度为50℃，PH值为4；② Pre-nickel-plating treatment of NdFeB thin-sheet magnetic steel products: the pre-nickel plating solution is composed of nickel sulfate, boric acid, sodium isethionate, hydroxypropyl sodium thiosulfate and water, and the mass volume concentration of nickel sulfate is 250 grams per liter, the mass volume concentration of boric acid is 40 grams per liter, the mass volume concentration of sodium isethionate is 20 mg/liter, and the mass volume concentration of hydroxypropyl sodium thiosulfate is 5 mg/liter. Nickel plating treatment time is 5000 seconds, double pulse power supply is used in the process of pre-nickel plating treatment, its forward current density is 0.6 ampere/square decimeter, reverse current density is 0.2 ampere/square decimeter, forward conduction time is 15 seconds, the reverse conduction time is 8 seconds, the forward frequency is 1.2kHz, the reverse frequency is 0.3kHz, the forward duty cycle is 60%, the reverse duty cycle is 20%, the temperature of the pre-nickel solution is 50 ℃, pH value is 4;
③采用去离子水对预镀镍处理过的钕铁硼薄片磁钢产品进行多次清洗，将预镀镍处理过的钕铁硼薄片磁钢产品清洗干净；清洗次数根据现有常规的电镀工艺选择，将表面残留的镀液清洗干净即可；③ Use deionized water to clean the pre-nickel-plated NdFeB thin-slice magnet products several times, and clean the pre-nickel-plated NdFeB thin-slice magnet products; the number of cleanings is based on the existing conventional electroplating process Select, just clean the residual plating solution on the surface;
④对钕铁硼薄片磁钢产品进行镀半光镍处理：半光镍溶液由硫酸镍、氯化镍、硼酸、酒石酸钾钠、三乙醇胺、硫酸铵、氨水和水组成，硫酸镍的质量体积浓度为150克/升，氯化镍的质量体积浓度为30克/升，硼酸的质量体积浓度为30克/升，酒石酸钾钠质量体积浓度为55克/升，三乙醇胺质量体积浓度为40克/升，硫酸铵质量体积浓度为30克/升，氨水体积百分比浓度为40毫升/升，镀半光镍处理时间为4500秒，镀半光镍处理过程中采用高频直流电源，其电流密度为0.5安培/平方分米，温度为50℃，PH值为5.5；④ Plating semi-bright nickel on NdFeB thin-sheet magnetic steel products: semi-bright nickel solution consists of nickel sulfate, nickel chloride, boric acid, potassium sodium tartrate, triethanolamine, ammonium sulfate, ammonia water and water, the mass volume of nickel sulfate Concentration is 150 grams/liter, and the mass volume concentration of nickel chloride is 30 grams/liter, and the mass volume concentration of boric acid is 30 grams/liter, and potassium sodium tartrate mass volume concentration is 55 grams/liter, and triethanolamine mass volume concentration is 40 gram/liter, the mass volume concentration of ammonium sulfate is 30 grams/liter, the volume percent concentration of ammonia water is 40 milliliters/liter, the treatment time of semi-gloss nickel plating is 4500 seconds, and high-frequency direct current power is adopted in the treatment process of semi-gloss nickel, and its current The density is 0.5 ampere/square decimeter, the temperature is 50°C, and the pH value is 5.5;
⑤采用去离子水对镀半光镍处理过的钕铁硼薄片磁钢产品进行多次清洗，将镀半光镍处理过的钕铁硼薄片磁钢产品清洗干净；清洗次数根据现有常规的电镀工艺选择，将表面残留的镀液清洗干净即可；⑤ Use deionized water to clean the semi-bright nickel-plated NdFeB thin-sheet magnet products several times, and clean the semi-bright nickel-plated NdFeB thin-sheet magnet products; the number of cleanings is based on the existing conventional Electroplating process selection, just clean the remaining plating solution on the surface;
⑥对钕铁硼薄片磁钢产品进行镀光亮镍处理：光亮镍溶液由硫酸镍、氯化镍、硼酸、糖精钠和水组成，硫酸镍的质量体积浓度为150克/升，氯化镍的质量体积浓度为50克/升，硼酸的质量体积浓度为45克/升，糖精钠的质量体积浓度为15毫克/升，镀光亮镍处理时间为3000秒，镀光亮镍处理过程中采用高频直流电源，其电流密度为0.5安培/平方分米，光亮镍溶液的温度为50℃，PH值为4；⑥ Perform bright nickel plating treatment on NdFeB thin-sheet magnetic steel products: the bright nickel solution is composed of nickel sulfate, nickel chloride, boric acid, sodium saccharin and water, the mass volume concentration of nickel sulfate is 150 g/L, and the The mass volume concentration is 50 g/l, the mass volume concentration of boric acid is 45 g/l, the mass volume concentration of saccharin sodium is 15 mg/l, the bright nickel plating treatment time is 3000 seconds, and high frequency is used in the bright nickel plating process DC power supply, its current density is 0.5 ampere/square decimeter, the temperature of bright nickel solution is 50 ℃, and the pH value is 4;
⑦采用去离子水对镀光亮镍处理过的钕铁硼薄片磁钢产品进行多次清洗，将镀光亮镍处理过的钕铁硼薄片磁钢产品清洗干净后烘干。⑦ Use deionized water to clean the bright nickel-plated NdFeB thin-slice magnet products several times, clean and dry the bright nickel-plated NdFeB thin-slice magnet products.
本实施例中，步骤①中前处理工艺包括以下步骤：In the present embodiment, the pretreatment process in step 1. includes the following steps:
①-1酸洗：采用稀硝酸溶液作为酸洗液对钕铁硼薄片磁钢产品进行酸洗；①-1 Pickling: Use dilute nitric acid solution as the pickling solution to pickle the NdFeB thin sheet magnet products;
①-2水洗：采用去离子水对酸洗后的钕铁硼薄片磁钢产品进行多次清洗，将表面残留的酸洗液清洗干净；①-2 Washing: Use deionized water to wash the pickled NdFeB thin sheet magnet products several times, and clean the residual pickling solution on the surface;
①-3将水洗后的钕铁硼薄片磁钢产品放入电解槽中进行电解处理，电解处理时间为300秒，电解液由氢氧化钠、碳酸钠、三聚磷酸钠和水组成，氢氧化钠的质量体积浓度为45克/升，碳酸钠的质量体积浓度为30克/升，三聚磷酸钠的质量体积浓度为30克/升，电解处理过程中电流密度为0.6安培/平方分米，电解液温度为40℃；①-3 Put the washed NdFeB thin sheet magnetic steel products into the electrolytic tank for electrolytic treatment. The electrolytic treatment time is 300 seconds. The electrolyte is composed of sodium hydroxide, sodium carbonate, sodium tripolyphosphate and water. The mass volume concentration of sodium is 45 grams/liter, the mass volume concentration of sodium carbonate is 30 grams/liter, the mass volume concentration of sodium tripolyphosphate is 30 grams/liter, and the current density during electrolytic treatment is 0.6 ampere/square decimeter , the electrolyte temperature is 40°C;
①-4水洗：采用去离子水对电解后的钕铁硼薄片磁钢产品进行多次清洗，将表面残留的电解液清洗干净。①-4Washing: Use deionized water to wash the electrolyzed NdFeB thin sheet magnet products several times to clean the residual electrolyte on the surface.
采用本实施例的方法对厚度为0.900±0.010毫米、端面积为2.88平方厘米、周长为7.95厘米、轮廓度为0.28、倒角值为0.25的钕铁硼薄片磁钢产品进行处理，薄片磁钢产品具体结构如图1所示。将上述钕铁硼薄片磁钢产品分成A组、B组和C组三组，分别采用本实施例的方法进行电镀镍处理，相应得到A组、B组和C组三组电镀镍后的产品。对A组、B组和C组三组电镀镍后的产品的镀层分布均匀性进行检测，其中镀层分布均匀性为产品尖端部与产品中心部镀层厚度的比值，比值越小，镀层分布均匀性越好。A组、B组和C组三组产品镀层分布均匀性：钕铁硼薄片磁钢产品的B点(即产品尖端部)镀层厚度与A点(即产品中心部)镀层厚度的比值如下表3所示。Adopt the method of this embodiment to process the neodymium-iron-boron thin sheet magnetic steel products with a thickness of 0.900 ± 0.010 mm, an end area of 2.88 square centimeters, a circumference of 7.95 cm, a contour of 0.28, and a chamfer value of 0.25. The specific structure of steel products is shown in Figure 1. Divide the above-mentioned NdFeB thin sheet magnetic steel products into three groups of A group, B group and C group, respectively adopt the method of this embodiment to carry out nickel plating treatment, and obtain the products of A group, B group and C group three groups after electroplating nickel correspondingly . The coating distribution uniformity of the nickel-plated products in Group A, Group B and Group C is tested. The uniformity of coating distribution is the ratio of the thickness of the coating at the tip of the product to the center of the product. The smaller the ratio, the more uniform the coating distribution. the better. The uniformity of the coating distribution of the three groups of products in Group A, Group B and Group C: the ratio of the thickness of the coating at point B (that is, the tip of the product) of the NdFeB thin sheet magnet product to the thickness of the coating at point A (that is, the center of the product) is shown in Table 3 shown.
表3table 3
分析表2数据可知，采用本实施例的方法处理的钕铁硼薄片磁钢产品的镀层分布均匀性优良。From the analysis of the data in Table 2, it can be known that the NdFeB flake magnet products processed by the method of this embodiment have excellent coating distribution uniformity.
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| CN (1) | CN105220194A (en) |
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| CN109056001A (en) * | 2018-10-24 | 2018-12-21 | 天津京磁电子元件制造有限公司 | Neodymium iron boron nickel plating solution and preparation method thereof, application method and plated item |
| CN110592623A (en) * | 2019-09-05 | 2019-12-20 | 宁波韵升股份有限公司 | Electroplating nickel solution formulation and method for improving uniform distribution of neodymium-iron-boron magnet coating |
| CN111074305A (en) * | 2020-01-14 | 2020-04-28 | 江西理工大学 | Method for depositing Ni layer on surface of magnetic steel based on double-pulse technology |
| CN112626577A (en) * | 2020-12-01 | 2021-04-09 | 中国兵器工业第五九研究所 | Preparation method of quartz crystal electrode film |
| CN113186573A (en) * | 2021-04-30 | 2021-07-30 | 东莞市环侨金属制品有限公司 | Manufacturing process of electroplated communication terminal |
| CN113279032A (en) * | 2021-04-30 | 2021-08-20 | 东莞市环侨金属制品有限公司 | Continuous electroplating process for metal product |
| CN114318479A (en) * | 2021-12-17 | 2022-04-12 | 宁波韵升股份有限公司 | Cleaning process of nickel-electroplated ultrathin magnetic steel |
| CN115522240A (en) * | 2022-10-31 | 2022-12-27 | 成都宏明双新科技股份有限公司 | A kind of pulse mist nickel plating process |
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| CN109056001A (en) * | 2018-10-24 | 2018-12-21 | 天津京磁电子元件制造有限公司 | Neodymium iron boron nickel plating solution and preparation method thereof, application method and plated item |
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| CN110592623A (en) * | 2019-09-05 | 2019-12-20 | 宁波韵升股份有限公司 | Electroplating nickel solution formulation and method for improving uniform distribution of neodymium-iron-boron magnet coating |
| CN110592623B (en) * | 2019-09-05 | 2021-01-05 | 宁波韵升股份有限公司 | Formula and method of nickel electroplating solution for improving uniform distribution of neodymium iron boron magnet coating |
| CN111074305A (en) * | 2020-01-14 | 2020-04-28 | 江西理工大学 | Method for depositing Ni layer on surface of magnetic steel based on double-pulse technology |
| CN112626577A (en) * | 2020-12-01 | 2021-04-09 | 中国兵器工业第五九研究所 | Preparation method of quartz crystal electrode film |
| CN112626577B (en) * | 2020-12-01 | 2023-05-19 | 中国兵器工业第五九研究所 | Preparation method of quartz crystal electrode film |
| CN113186573A (en) * | 2021-04-30 | 2021-07-30 | 东莞市环侨金属制品有限公司 | Manufacturing process of electroplated communication terminal |
| CN113279032A (en) * | 2021-04-30 | 2021-08-20 | 东莞市环侨金属制品有限公司 | Continuous electroplating process for metal product |
| CN114318479A (en) * | 2021-12-17 | 2022-04-12 | 宁波韵升股份有限公司 | Cleaning process of nickel-electroplated ultrathin magnetic steel |
| CN115522240A (en) * | 2022-10-31 | 2022-12-27 | 成都宏明双新科技股份有限公司 | A kind of pulse mist nickel plating process |
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