WO2024087548A1 - 永磁体的表面处理方法、永磁体及其保护膜 - Google Patents

永磁体的表面处理方法、永磁体及其保护膜 Download PDF

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WO2024087548A1
WO2024087548A1 PCT/CN2023/090163 CN2023090163W WO2024087548A1 WO 2024087548 A1 WO2024087548 A1 WO 2024087548A1 CN 2023090163 W CN2023090163 W CN 2023090163W WO 2024087548 A1 WO2024087548 A1 WO 2024087548A1
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permanent magnet
treatment
time
zirconization
agent
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PCT/CN2023/090163
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English (en)
French (fr)
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张艳艳
梁亚岷
傅东辉
赖火秀
黄佳莹
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福建省金龙稀土股份有限公司
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Publication of WO2024087548A1 publication Critical patent/WO2024087548A1/zh

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    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/78—Pretreatment of the material to be coated
    • C23C22/80—Pretreatment of the material to be coated with solutions containing titanium or zirconium compounds
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
    • C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
    • C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
    • H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets

Definitions

  • the invention relates to a surface treatment method of a permanent magnet, a permanent magnet and a protective film thereof.
  • Permanent magnet material is a porous material prepared by powder metallurgy process. Because of the neodymium-rich phase, neodymium iron boron main phase and boundary phase, it is easy to form intergranular corrosion. In humid air, the magnet mainly fails due to oxidation and fracture of crystal particles, which eventually leads to the decline or damage of the magnetic properties of the material, seriously affecting the service life of the permanent magnet and reducing the stability and reliability of the product.
  • the traditional ternary phosphating pretreatment materials for coating are gradually banned by local regulations due to the presence of pollutants such as P, Mn, Ni, etc.
  • the new green phosphorus-free conversion film technology has gradually matured and developed rapidly. This process can completely avoid the use of harmful substances such as P, Mn, Ni, nitrite, etc.
  • the coating surface prepared by the existing zirconium salt pretreatment process is uneven, the corrosion resistance is not high, and after high temperature and high pressure test, wet heat test and neutral salt spray test, its anti-corrosion effect is poor.
  • the protective film has better protection in conventional environments and high temperature and high humidity environments, that is, good moisture resistance, but also has good surface tension to meet the requirements of subsequent processing.
  • the preparation process has large pollution and other defects, and provides a surface treatment method, a permanent magnet and a protective film thereof.
  • the permanent magnet obtained has good moisture resistance and large surface tension; the treatment method of the present invention reduces pollutant emissions and conforms to the green ecological and environmental protection production concept.
  • the present invention solves the above technical problems through the following technical solutions.
  • the present invention provides a surface treatment method for a permanent magnet, which comprises the following steps:
  • the zirconization treatment is performed by immersing the permanent magnet in an aqueous solution containing a zirconization agent.
  • the zirconizing agent can be a conventional zirconizing agent in the art; preferably, the zirconizing agent includes fluorozirconate and/or fluorozirconic acid; more preferably, the zirconizing agent is a special zirconizing agent for rare earth neodymium iron boron materials, which comes from Hainan Hongxiang Industrial Co., Ltd.
  • the concentration of the aqueous solution containing the zirconizing agent is 10%-60%, and the concentration of the aqueous solution containing the zirconizing agent is the mass percentage of the zirconizing agent in the aqueous solution containing the zirconizing agent.
  • the immersion may be direct immersion or indirect immersion.
  • the direct immersion refers to immersing the permanent magnet in the aqueous solution containing the zirconizing agent.
  • the indirect immersion is preferably drum immersion.
  • the drum immersion refers to placing the permanent magnet in a drum and then immersing it in the aqueous solution containing the zirconizing agent, and rotating the drum during the treatment process so that all surfaces of the permanent magnet are fully in contact with the zirconizing agent.
  • the temperature of the zirconization treatment is 20-30°C.
  • the zirconization treatment time is 10-25 min, more preferably 15 min-20 min.
  • the adhesion effect of the zirconization film on the permanent magnet is related to the concentration of the aqueous solution containing the zirconization agent, the pH value, temperature, time of the zirconization treatment and the cleanliness of the permanent magnet surface.
  • the permanent magnet with the zirconium film is sequentially washed and dried for a third time.
  • the third washing time is 10-20 seconds.
  • the overflow water flow rate of the third water washing is 100 cubic meters per hour.
  • the drying temperature is 80°C.
  • the drying time is 30 minutes.
  • the passivation treatment is physical passivation; compared with other passivation processes, the passivation treatment of the present invention can be performed at a lower temperature.
  • the passivation treatment is carried out in an aqueous solution containing a passivating agent.
  • the passivator can be a conventional passivator in the art, preferably a mixture of weakly acidic organic acid salts and inorganic salts; wherein, the organic acid salt preferably includes one or more of trisodium citrate, sodium salicylate and tetrasodium EDTA; preferably, the inorganic salt is preferably barium titanate; more preferably, the passivator includes trisodium citrate, sodium salicylate, tetrasodium EDTA and barium titanate.
  • the concentration of the aqueous solution containing the passivator is 10%-20%, and the concentration of the aqueous solution containing the passivator is the mass percentage of the passivator in the aqueous solution containing the passivator.
  • the temperature of the passivation treatment is 25-50°C, more preferably 25-30°C.
  • the passivation treatment time is 6-10 min, more preferably 8-10 min.
  • the passivation treatment is achieved by immersing or spraying; the immersion refers to immersing the permanent magnet in an aqueous solution containing a passivator; the spraying refers to spraying the aqueous solution containing a passivator on the permanent magnet.
  • the drying temperature is 70-90°C, more preferably 75-85°C.
  • the drying time is 25-40 minutes, more preferably 25-35 minutes.
  • the preparation process includes zirconization treatment and passivation treatment; after the zirconization treatment, a layer of locally dense zirconization film will be formed on the surface of the permanent magnet, but dried cracks will appear on its surface; the passivation film formed after the passivation treatment can cover its surface to form a closed layer, which will not damage the zirconization film, but can also seal and fill the defects or weak points of the zirconization film and repair the cracks of the zirconization film.
  • the above inner and outer layers cooperate with each other to form a moisture-resistant protective film.
  • the aqueous solution containing the zirconizing agent is acidic, and the aqueous solution containing the passivating agent is alkaline. During the treatment process, mutual contamination between the two needs to be avoided.
  • the permanent magnet may be pretreated before the zirconization treatment; wherein, preferably, the pretreatment steps include in sequence: 1 grinding; 2 degreasing; 3 first water washing; 4 pickling and rust removal; 5 second water washing; 6 ultrasonic deashing.
  • step 1 the grinding can be a conventional operation in the art.
  • step 1 preferably, a rust inhibitor is added during the grinding process.
  • the rust inhibitor can be a conventional rust inhibitor in the art; preferably, the rust inhibitor includes one or more of sodium phosphate, sodium carbonate, sodium hydroxide and OP-10 emulsifier; more preferably, the concentration of sodium phosphate is 60-80g/L, sodium carbonate is 40-60g/L, sodium hydroxide is 5-10g/L or OP-10 emulsifier is 0.05-1g/L.
  • step 1 preferably, the grinding is carried out in a vibrating grinder.
  • step 1 preferably, the grinding temperature is 10-40°C.
  • step 1 preferably, the grinding time is 2-36h.
  • step 2 the degreasing can be a conventional operation in the art.
  • step 2 preferably, degreasing powder is added during the degreasing process.
  • the degreasing powder may be conventional degreasing powder in the art.
  • step 2 preferably, the degreasing temperature is 45-55°C.
  • step 2 preferably, the degreasing time is 3-7 minutes.
  • step 3 the first water washing can be a conventional operation in the art.
  • step 3 preferably, the first water washing is carried out in the first water washing tank and the second water washing tank respectively.
  • the first washing time is 10-20 seconds.
  • step 3 preferably, the overflow water flow rate of the first water wash is 100 cubic meters per hour.
  • step 4 preferably, the pickling and rust removal time is 30-50s.
  • the acid used for pickling and rust removal is dilute nitric acid; more preferably, the concentration of the dilute nitric acid is 1%-3%.
  • step 4 the pickling and rust removal is to remove the oxide layer on the surface of the permanent magnet, so as to facilitate the subsequent zirconization film to better cover the surface of the permanent magnet.
  • step 5 the first water washing can be a conventional operation in the art.
  • step 5 preferably, the second water washing is carried out in the third water washing tank.
  • step 5 preferably, the second washing time is 10-20 seconds.
  • step 5 preferably, the overflow water flow rate of the second water washing is 100 cubic meters per hour.
  • step 6 preferably, the ultrasonic deashing is carried out in the fourth water washing tank.
  • step 6 preferably, an ultrasonic protective agent is added before the ultrasonic deashing.
  • adding an ultrasonic protective agent can achieve a better ultrasonic effect, and the magnet surface is more clean, which is conducive to subsequent film formation.
  • the ultrasonic protective agent is a conventional ultrasonic protective agent in the art; preferably, the concentration of the ultrasonic protective agent is 0.1-1%, and the concentration of the ultrasonic protective agent is the mass percentage of the ultrasonic protective agent in the washing water of the fourth washing tank.
  • step 6 preferably, the ultrasonic deashing time is 2-5 minutes.
  • the present invention also provides a permanent magnet, which is obtained by using the surface treatment method of the permanent magnet as described above.
  • the present invention also provides a permanent magnet protective film, which is obtained by the surface treatment method of the permanent magnet as described above.
  • the reagents and raw materials used in the present invention are commercially available.
  • a chemically extremely stable protective film can be formed on the surface of the NdFeB material in a short time.
  • the protective film has excellent corrosion resistance, dense and uniform film crystals, and good rust resistance.
  • AHT test alternating air temperature and humidity
  • the protective film on the surface of the permanent magnet obtained by the process of the present invention also has a large Surface tension provides good adhesion in subsequent permanent magnet applications.
  • the process of the present invention is in line with the green ecological and environmental protection production concept, avoiding the problem of sediment and the emission of a large amount of pollutants.
  • FIG1 is a sample diagram of the product prepared in Example 1 before and after being tested in a wet heat chamber for 15 cycles (360 h).
  • FIG. 2 is a sample diagram of the product prepared in Comparative Example 1 before and after being tested in a wet heat chamber for 4 cycles (96 hours).
  • FIG3 is a sample diagram of the product prepared in Comparative Example 2 before and after being tested in a wet heat chamber for 5 cycles (120 h).
  • This embodiment is a surface treatment method for a permanent magnet, which comprises the following steps:
  • pre-processing the permanent magnet comprises the following steps:
  • the permanent magnet into a vibration grinder and add a rust inhibitor for grinding.
  • the grinding temperature is 25°C and the grinding time is 10 hours.
  • the rust inhibitor is 70g/L sodium phosphate, 50g/L sodium carbonate and 8g/L sodium hydroxide.
  • the first water washing time is 20s, and the overflow water flow rate of the first water washing is 100 cubic meters per hour;
  • the second water washing time is 10s, and the overflow water flow rate of the second water washing is 100 cubic meters per hour;
  • the ultrasonic deashing time is 4 minutes, the concentration of the ultrasonic protective agent is 0.5%, and the concentration of the ultrasonic protective agent is the mass percentage of the ultrasonic protective agent in the washing water of the fourth water washing tank;
  • the concentration of the zirconizing agent is the mass percentage of the zirconizing agent in the aqueous solution containing the zirconizing agent;
  • the zirconizing agent is a special zirconizing agent for rare earth neodymium iron boron materials, which comes from Hainan Hongxiang Industrial Co., Ltd. and includes fluorozirconate and fluorozirconic acid;
  • the zirconized permanent magnet is washed and dried for the third time in sequence; the third washing time is 15 seconds; the overflow water flow of the third washing is 100 cubic meters per hour; the drying temperature is 80° C.; and the drying time is 30 minutes;
  • the zirconizing agent is immersed in a passivating agent with a concentration of 20% for 8 minutes at 25°C and a pH value greater than or equal to 10, and then dried at a temperature of 80°C for 30 minutes; the zirconizing agent is a mixture of trisodium citrate, sodium salicylate, tetrasodium EDTA and barium titanate.
  • the permanent magnet is pretreated by adopting step S0 in embodiment 1;
  • the concentration of the zirconizing agent is the mass percentage of the zirconizing agent in the aqueous solution containing the zirconizing agent;
  • the zirconizing agent is a special zirconizing agent for rare earth neodymium iron boron materials, which comes from Hainan Hongxiang Industrial Co., Ltd. and includes fluorozirconate and fluorozirconic acid;
  • the zirconized permanent magnet is successively washed with water for the third time and dried. drying; the third washing time is 10 seconds; the overflow water flow of the third washing is 100 cubic meters per hour; the drying temperature is 80°C; the drying time is 30 minutes;
  • a passivation treatment is carried out by spraying in a passivating agent with a concentration of 20% at 50° C. and a pH value of 10 for 4 minutes, and then drying is carried out at a temperature of 80° C. for 30 minutes;
  • the zirconizing agent is a mixture of trisodium citrate, sodium salicylate, tetrasodium EDTA and barium titanate.
  • the permanent magnet is pretreated by adopting step S0 in embodiment 1;
  • the concentration of the zirconizing agent is the mass percentage of the zirconizing agent in the aqueous solution containing the zirconizing agent;
  • the zirconizing agent is a special zirconizing agent for rare earth neodymium iron boron materials, which comes from Hainan Hongxiang Industrial Co., Ltd. and includes fluorozirconate and fluorozirconic acid;
  • the zirconized permanent magnet is sequentially washed and dried for the third time; the time of the third washing is 20 seconds; the overflow water flow of the third washing is 100 cubic meters per hour; the drying temperature is 80° C.; and the drying time is 30 minutes;
  • the passivation treatment is carried out by immersion or spraying in a passivating agent with a concentration of 20% at 15°C and a pH value of 10 for 12 minutes, and then drying is carried out at a temperature of 80°C for 30 minutes;
  • the zirconizing agent is a mixture of trisodium citrate, sodium salicylate, tetrasodium EDTA and barium titanate.
  • the existing phosphating process is adopted to perform phosphating treatment on the surface of the permanent magnet to obtain the permanent magnet.
  • Example 1 The treatment method of Example 1 is adopted.
  • the difference between this comparative example and Example 1 is that the temperature of the zirconization treatment in step S1 is 50° C., and the time of the zirconization treatment is 40 minutes.
  • Example 1 The treatment method of Example 1 is adopted. The difference between this comparative example and Example 1 is that the pH value of the zirconization treatment in step S1 is 7.
  • Step S2 The temperature of the passivation treatment is 10° C., and the time of the passivation treatment is 10 min.
  • Example 1 The treatment method of Example 1 is adopted. The difference between this comparative example and Example 1 is that the pH value of the passivation treatment in step S2 is 9.
  • Figure 1 is a sample diagram of the product prepared in Example 1 before and after 15 cycles (360 hours) of the wet heat box test
  • Figure 1 (a) is a sample diagram before the test
  • Figure 1 (b) is a sample diagram after the test.
  • the moisture resistance time of the permanent magnet of Example 1 can reach more than 15 cycles (360 hours), and the appearance does not change color or have rust spots after the test.
  • Figure 2 is a sample diagram of the permanent magnet prepared in Comparative Example 1 before and after being tested in a wet heat box for 4 cycles (96 hours)
  • Figure 2 (a) is a sample diagram before the test
  • Figure 2 (b) is a sample diagram after the test.
  • Figure 3 is a sample diagram of the permanent magnet prepared in Comparative Example 2 before and after being tested in a wet heat box for 5 cycles (120 hours)
  • Figure 3 (a) is a sample diagram before the test
  • Figure 3 (b) is a sample diagram after the test. After the permanent magnet of Comparative Example 2 was tested in a wet heat box for 5 cycles (120 hours), obvious red rust spots appeared on the surface.
  • the surface tension of the permanent magnet moisture-resistant protective film prepared by the treatment method of the present application can reach 40 mN/m or above.

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Abstract

本发明公开了永磁体的表面处理方法、永磁体及其保护膜。永磁体的表面处理方法包括以下步骤：S1、将永磁体进行锆化处理，得到具有锆化膜的永磁体；锆化处理的温度为5-40℃，时间为5-30min，锆化处理的pH值为1.5-6；S2、将具有锆化膜的永磁体进行钝化处理，烘干即可；钝化处理的温度为15-50℃，时间4-12min，pH值大于等于10。通过本发明的处理方法，得到的永磁体具有较好的耐湿性，并同时具有较大的表面张力；本发明的处理方法减少了污染物排放，符合绿色生态环保生产理念。

Description

永磁体的表面处理方法、永磁体及其保护膜 技术领域
本发明涉及一种永磁体的表面处理方法、永磁体及其保护膜。
背景技术
永磁材料是一种粉末冶金工艺制备而成的多孔材料，因其中的富钕相、钕铁硼主相及边界相很容易形成晶间腐蚀。磁体在潮湿的空气主要是晶体颗粒被氧化而断裂造成失效，最终导致材料的磁性能下降或损坏，严重影响了永磁体的使用寿命，降低了产品的稳定性和可靠性。
随着国内外对节能、环保及污水排放要求的不断提高，传统的涂装三元磷化前处理材料因含有P、Mn、Ni等污染物逐渐被地方法规禁止，新型的绿色无磷转化膜技术逐渐成熟并快速发展，该工艺能彻底地不使用P、Mn、Ni、亚硝酸根等有害物质。然而，采用现有的锆盐前处理工艺所制得的涂层表面不均匀，耐蚀性不高，且经过高温高压试验、湿热试验和中性盐雾试验后，其防腐蚀效果较差。
另外，在汽车领域应用中，磁体需要使用胶水与其他工件进行粘接拼装。为此这一类应用中对磁体表面防护膜的亲胶性具有更高的要求。比如，当前在车载音响中，磁体的表面张力需要达到38mN/m以上才能满足组装时的黏胶需求。然而常规有机涂层虽具有一定的耐湿性，但其表面能较低，从而导致镀层的表面张力难以达到较高水平。
因此，在钕铁硼表面制备保护膜，不仅需要考虑保护膜在常规环境和高温、高湿环境中防护性较佳，即耐湿性能好，还要具有良好的表面张力，满足后续加工的要求。
发明内容
为了克服现有技术中永磁体材料难以同时具有较好的耐湿性和表面张 力，且制备工艺的污染较大等缺陷，而提供了一种表面的处理方法、永磁体及其保护膜。通过本发明的处理方法，得到的永磁体具有较好的耐湿性，并同时具有较大的表面张力；本发明的处理方法减少了污染物排放，符合绿色生态环保生产理念。
本发明通过下述技术方案来解决上述技术问题。
本发明提供了一种永磁体的表面处理方法，其包括以下步骤：
S1、将永磁体进行锆化处理，得到具有锆化膜的永磁体；所述锆化处理的温度为5-40℃，所述锆化处理的时间为5-30min；所述锆化处理的pH值为1.5-6；
S2、将所述具有锆化膜的永磁体进行钝化处理，烘干即可；所述钝化处理的温度为15-50℃，所述钝化处理的时间4-12min，所述钝化处理的pH值大于等于10。
S1中，较佳地，所述锆化处理通过将所述永磁体浸泡在含锆化剂的水溶液中进行。
其中，所述锆化剂可为本领域常规的锆化剂；较佳地，所述锆化剂包括氟锆酸盐和/或氟锆酸；更佳地，所述锆化剂为稀土钕铁硼材料专用锆化剂，来自海南鸿翔实业有限公司。
其中，较佳地，所述含锆化剂的水溶液的浓度为10％-60％，所述含锆化剂的水溶液的浓度为锆化剂占所述含锆化剂的水溶液的质量百分比。
其中，所述浸泡可为直接浸泡或间接浸泡。所述直接浸泡是指将永磁体浸入所述含锆化剂的水溶液中。所述间接浸泡优选为滚筒浸泡。所述滚筒浸泡是指将永磁体放入滚筒中再浸泡在含锆化剂的水溶液中，处理过程中转动滚筒，让永磁体的各个面都与锆化剂充分接触。
S1中，较佳地，所述锆化处理的温度为20-30℃。
S1中，较佳地，所述锆化处理的时间为10-25min，更佳地为15min-20min。
S1中，所述锆化膜在永磁体上的附着效果与含锆化剂的水溶液的浓度、锆化处理的pH值、温度、时间和永磁体表面洁净度有关。
S2中，较佳地，在所述钝化处理前，所述具有锆化膜的永磁体依次经过第三次水洗和干燥。
其中，较佳地，所述第三次水洗的时间为10-20秒。
其中，较佳地，所述第三次水洗的溢流水流量为100立方/小时。
其中，较佳地，所述干燥的温度为80℃。
其中，较佳地，所述干燥的时间为30min。
S2中，所述钝化处理为物理钝化；相比其他钝化工艺，本发明的钝化处理可在较低的温度下进行。
S2中，较佳地，所述钝化处理在含钝化剂的水溶液中进行。
其中，所述钝化剂可为本领域常规的钝化剂，较佳地为呈弱酸性的有机酸盐和无机盐的混合物；其中，所述有机酸盐较佳地包括柠檬酸三钠、水杨酸钠和EDTA四钠中的一种或多种；较佳地，所述无机盐较佳地为钛酸钡；更佳地，所述钝化剂包括柠檬酸三钠、水杨酸钠、EDTA四钠和钛酸钡。
其中，较佳地，所述含钝化剂的水溶液的浓度为10％-20％，所述含钝化剂的水溶液的浓度为钝化剂占所述含钝化剂的水溶液的质量百分比。
S2中，较佳地，所述钝化处理的温度为25-50℃，更佳地为25-30℃。
S2中，较佳地，所述钝化处理的时间为6-10min，更佳地为8-10min。
S2中，较佳地，所述钝化处理通过浸泡或喷洒实现；所述浸泡是指将永磁体浸入含钝化剂的水溶液中；所述喷洒是指将含钝化剂的水溶液喷洒在永磁体上。
S2中，较佳地，所述烘干的温度为70-90℃，较佳地为75-85℃。
S2中，较佳地，所述烘干的时间为25-40min，较佳地为25-35min。
本发明中，所述制备工艺包括锆化处理和钝化处理；经过所述锆化处理后，永磁体表面会形成一层局部致密的锆化膜，但其表面会出现干涸的裂纹；经过钝化处理后形成的钝化膜能覆盖于其表面，形成封闭层，其既不会损害锆化膜，还可封闭填充锆化膜的缺陷或薄弱处，修复锆化膜的裂纹。上述内外两层膜相互配合而形成了耐湿性保护膜。
本发明中，所述含锆化剂的水溶液呈酸性，所述含钝化剂的水溶液呈碱性，在处理过程中，需避免两者的相互污染。
本发明中，在所述锆化处理之前可对永磁体进行预处理；其中，较佳地，所述预处理的步骤依次包括：①研磨；②脱脂；③第一次水洗；④酸洗除锈；⑤第二次水洗；⑥超声去灰。
步骤①中，所述研磨可为本领域常规操作。
步骤①中，较佳地，在所述研磨的过程中加入防锈剂。
其中，所述防锈剂可为本领域常规的防锈剂；较佳地，所述防锈剂包括磷酸钠、碳酸钠、氢氧化钠和OP-10乳化剂中的一种或多种；更佳地，所述磷酸钠的浓度为60-80g/L，碳酸钠40-60g/L，氢氧化钠5-10g/L或OP-10乳化剂0.05-1g/L中的一种或多种。
步骤①中，较佳地，所述研磨在振动式研磨机中进行。
步骤①中，较佳地，所述研磨的温度为10-40℃。
步骤①中，较佳地，所述研磨的时间为2-36h。
步骤②中，所述脱脂可为本领域常规操作。
步骤②中，较佳地，在所述脱脂的过程中加入除油粉。
其中，所述除油粉可为本领域常规的除油粉。
步骤②中，较佳地，所述脱脂的温度为45-55℃。
步骤②中，较佳地，所述脱脂的时间为3-7min。
步骤③中，所述第一次水洗可为本领域常规操作。
步骤③中，较佳地，所述第一次水洗分别在第一水洗槽和第二水洗槽中进行。
步骤③中，较佳地，所述第一次水洗的时间为10-20秒。
步骤③中，较佳地，所述第一次水洗的溢流水流量为100立方/小时。
步骤④中，较佳地，所述酸洗除锈的时间为30-50s。
步骤④中，较佳地，所述酸洗除锈的酸为稀硝酸；更佳地，所述稀硝酸的浓度为1％-3％。
步骤④中，所述酸洗除锈是为了去除永磁体表面的氧化层，以利于后续锆化膜更好的覆着在永磁体表面。
步骤⑤中，所述第一次水洗可为本领域常规操作。
步骤⑤中，较佳地，所述第二次水洗在第三水洗槽中进行。
步骤⑤中，较佳地，所述第二次水洗的时间为10-20秒。
步骤⑤中，较佳地，所述第二次水洗的溢流水流量为100立方/小时。
步骤⑥中，较佳地，所述超声去灰在第四水洗槽中进行。
步骤⑥中，较佳地，进行所述超声去灰前，加入超声保护剂。在所述超声去灰的过程中，加入超声保护剂，可达到较好的超声效果，磁体表面洁净度更高，利于后续成膜。
其中，所述超声保护剂为本领域常规的超声保护剂；较佳地，所述超声保护剂的浓度为0.1-1％，所述超声保护剂的浓度为超声保护剂占所述第四水洗槽的洗涤水的质量百分比。
步骤⑥中，较佳地，所述超声去灰的时间为2-5min。
本发明还提供了一种永磁体，其采用如上所述的永磁体的表面处理方法得到。
本发明还提供了一种永磁体保护膜，其由如上所述的永磁体的表面处理方法得到。
在符合本领域常识的基础上，上述各优选条件，可任意组合，即得本发明各较佳实例。
本发明所用试剂和原料均市售可得。
本发明的积极进步效果在于：
1、采用本发明的工艺，可短时间内在钕铁硼材料表面形成化学性质极为稳定的保护膜，该保护膜具有优良耐蚀性，膜层结晶致密、均匀、防锈能力好。在空气温度和湿度交替变化冷凝试验中(AHT测试)，永磁体的耐湿时间达7个循环(168h)以上，且试验后外观不发生变色、无锈点。
2、采用本发明的工艺，得到的永磁体表面的保护膜同时还具有较大的 表面张力，在后续永磁体的应用中具有较好的粘结性。
3、采用本发明的工艺，符合绿色生态环保生产理念，避免了沉渣的问题和大量污染物的排放问题。
4、采用本发明的工艺，得到了锆化层和钝化层的双层结构的表面保护膜具有较佳的均匀性和外观一致性。
附图说明
图1为实施例1制得的产品经过湿热箱15个循环(360h)测试的前后样品图。
图2为对比例1制得的产品经过湿热箱4个循环(96h)测试的前后样品图。
图3为对比例2制得的产品经过湿热箱5个循环(120h)测试的前后样品图。
具体实施方式
下面通过实施例的方式进一步说明本发明，但并不因此将本发明限制在所述的实施例范围之中。下列实施例中未注明具体条件的实验方法，按照常规方法和条件，或按照商品说明书选择。
实施例1
本实施例为永磁体的表面处理方法，其包括以下步骤：
S0、对永磁体进行预处理包括如下步骤：
①将永磁体放入振动式研磨机中，同时加入防锈剂研磨，研磨的温度为25℃，研磨的时间为10h，防锈剂为70g/L的磷酸钠、50g/L的碳酸钠和8g/L的氢氧化钠；
②将研磨后的永磁体与除油粉混合，进行脱脂，脱脂的温度为50℃，脱脂的时间为5min；
③将脱脂后的永磁体依次置于第一水洗槽和第二水洗槽中进行第一次 水洗，第一次水洗的时间为20s，第一次水洗的溢流水流量为100立方/小时；
④使用浓度为3％的稀硝酸对第一次水洗后的永磁体进行酸洗除锈，酸洗除锈的时间为40s；
⑤将酸洗除锈后的永磁体置于第三水洗槽中进行第二次水洗，第二次水洗的时间为10s，第二次水洗的溢流水流量为100立方/小时；
⑥将第二次水洗后的永磁体置于第四水洗槽中，并加入超声保护剂进行超声去灰，超声去灰的时间为4min，超声保护剂的浓度为0.5％，超声保护剂的浓度为超声保护剂占第四水洗槽的洗涤水的质量百分比；
S1、将S0经预处理的永磁体置于浓度为50％的锆化剂中，在25℃、pH值为3.8的条件下锆化处理15min，通过浸泡涂覆得到锆化后的永磁体；锆化剂的浓度为锆化剂占含锆化剂的水溶液的质量百分比；该锆化剂为稀土钕铁硼材料专用锆化剂，来自海南鸿翔实业有限公司，其包括氟锆酸盐和氟锆酸；
S2、在所述钝化处理前，所述锆化后的永磁体依次经过第三次水洗和干燥；第三次水洗的时间为15秒；第三次水洗的溢流水流量为100立方/小时；干燥的温度为80℃；干燥的时间为30min；
随后，在25℃、pH值大于等于10的条件下在浓度为20％的钝化剂中进行浸泡钝化处理8min，在温度为80℃下烘干30min即可；该锆化剂为柠檬酸三钠、水杨酸钠、EDTA四钠和钛酸钡的混合物。
实施例2
采用实施例1中S0的步骤对永磁体进行预处理；
S1、将S0经预处理的永磁体置于浓度为50％的锆化剂中，在5℃、pH值为3.5的条件下锆化处理20min，通过浸泡涂覆得到锆化后的永磁体；锆化剂的浓度为锆化剂占含锆化剂的水溶液的质量百分比；该锆化剂为稀土钕铁硼材料专用锆化剂，来自海南鸿翔实业有限公司，其包括氟锆酸盐和氟锆酸；
S2、在所述钝化处理前，所述锆化后的永磁体依次经过第三次水洗和干 燥；第三次水洗的时间为10秒；第三次水洗的溢流水流量为100立方/小时；干燥的温度为80℃；干燥的时间为30min；
随后，在50℃、pH值为10的条件下在浓度为20％的钝化剂中进行喷洒的钝化处理4min，在温度为80℃下烘干30min即可；该锆化剂为柠檬酸三钠、水杨酸钠、EDTA四钠和钛酸钡的混合物。
实施例3
采用实施例1中S0的步骤对永磁体进行预处理；
S1、将S0经预处理的永磁体置于浓度为50％的锆化剂中，在40℃、pH值为3.5的条件下锆化处理5min，通过滚筒涂覆得到锆化后的永磁体；锆化剂的浓度为锆化剂占含锆化剂的水溶液的质量百分比；该锆化剂为稀土钕铁硼材料专用锆化剂，来自海南鸿翔实业有限公司，其包括氟锆酸盐和氟锆酸；
S2、在所述钝化处理前，所述锆化后的永磁体依次经过第三次水洗和干燥；第三次水洗的时间为20秒；第三次水洗的溢流水流量为100立方/小时；干燥的温度为80℃；干燥的时间为30min；
随后，在15℃、pH值为10的条件下在浓度为20％的钝化剂中进行浸泡或喷洒的钝化处理12min，在温度为80℃下烘干30min即可；该锆化剂为柠檬酸三钠、水杨酸钠、EDTA四钠和钛酸钡的混合物。
对比例1
采用现有的磷化工艺，对永磁体表面进行磷化处理，得到永磁体。
对比例2
采用如实施例1的处理方法，本对比例与实施例1的区别为：步骤S1中的锆化处理的温度为50℃，锆化处理的时间为40min。
对比例3
采用如实施例1的处理方法，本对比例与实施例1的区别为：步骤S1中的锆化处理的pH值为7。
对比例4
采用如实施例1的处理方法，本对比例与实施例1的区别为：步骤S2 中的钝化处理的温度为10℃，所述钝化处理的时间10min。
对比例5
采用如实施例1的处理方法，本对比例与实施例1的区别为：步骤S2中的钝化处理的pH值为9。
效果实施例1
AHT测试
将实施例1～3和对比例1～5的永磁体分别进行AHT测试，即在空气温度和湿度交替变化冷凝试验，得到的结果如图1～3和表1所示。
图1为实施例1制得的产品经过湿热箱15个循环(360h)测试的前后样品图，图1(a)为测试前的样品图，图1(b)为测试后的样品图。实施例1的永磁体的耐湿时间可达15个循环(360h)以上，且试验后外观不发生变色、无锈点。
图2为对比例1制得的永磁体经过湿热箱4个循环(96h)测试的前后样品图，图2(a)为测试前的样品图，图2(b)为测试后的样品图。对比例1的永磁体经过湿热箱4个循环(96h)后，表面虽无锈点，但出现了明显的变色，视为腐蚀失效前兆。
图3为对比例2制得的永磁体经过湿热箱5个循环(120h)测试的前后样品图，图3(a)为测试前的样品图，图3(b)为测试后的样品图。对比例2的永磁体经过湿热箱5个循环(120h)后，表面出现了明显的红色锈点。
表1

效果实施例2表面张力测试
使用本领域常规的达因笔测试判定方法测试实施例1-3和对比例1-5永磁体的表面张力，得到如表2所示的结果：
表2
可知，由本申请的处理方法制得的永磁体耐湿性保护膜的表面张力可达到40mN/m及以上。

Claims (10)

  1. 一种永磁体的表面处理方法，其特征在于，其包括以下步骤：
    S1、将永磁体进行锆化处理，得到具有锆化膜的永磁体；所述锆化处理的温度为5-40℃，所述锆化处理的时间为5-30min；所述锆化处理的pH值为1.5-6；
    S2、将所述具有锆化膜的永磁体进行钝化处理，烘干即可；所述钝化处理的温度为15-50℃，所述钝化处理的时间4-12min，所述钝化处理的pH值大于等于10。
  2. 如权利要求1所述的永磁体的表面处理方法，其特征在于，S1中，所述锆化处理通过将所述永磁体浸泡在含锆化剂的水溶液中进行；
    和/或，所述锆化处理的温度为20-30℃；
    和/或，所述锆化处理的时间为10-25min；
    和/或，所述锆化处理的pH为3.2-5.5。
  3. 如权利要求2所述的永磁体的表面处理方法，其特征在于，S1中，所述锆化剂包括氟锆酸盐和/或氟锆酸；
    和/或，所述含锆化剂的水溶液的浓度为10％-60％，所述含锆化剂的水溶液的浓度为锆化剂占所述含锆化剂的水溶液的质量百分比；
    和/或，所述浸泡为直接浸泡或间接浸泡；
    和/或，所述锆化处理的时间为15-20min。
  4. 如权利要求1所述的永磁体的表面处理方法，其特征在于，S2中，在所述钝化处理前，所述具有锆化膜的永磁体依次经过第三次水洗和干燥；
    和/或，所述钝化处理在含钝化剂的水溶液中进行；
    和/或，所述钝化处理的温度为25-50℃；
    和/或，所述钝化处理的时间为6-10min；
    和/或，所述钝化处理通过浸泡或喷洒实现；
    和/或，所述烘干的温度为70-90℃；
    和/或，所述烘干的时间为25-40min。
  5. 如权利要求4所述的永磁体的表面处理方法，其特征在于，S2中， 所述第三次水洗的时间为10-20秒；
    和/或，所述第三次水洗的溢流水流量为100立方/小时；
    和/或，所述干燥的温度为80℃；
    和/或，所述干燥的时间为30min；
    和/或，所述钝化剂为呈弱酸性的有机酸盐和无机盐的混合物；其中，所述有机酸盐较佳地包括柠檬酸三钠、水杨酸钠和EDTA四钠中的一种或多种；所述无机盐较佳地为钛酸钡；较佳地，所述钝化剂包括柠檬酸三钠、水杨酸钠、EDTA四钠和钛酸钡；
    和/或，所述含钝化剂的水溶液的浓度为10％-20％，所述含钝化剂的水溶液的浓度为钝化剂占所述含钝化剂的水溶液的质量百分比；
    和/或，所述钝化处理的温度为25-30℃；
    和/或，所述钝化处理的时间为8-10min；
    和/或，所述烘干的温度为75-85℃；
    和/或，所述烘干的时间为25-35min。
  6. 如权利要求1所述的永磁体的表面处理方法，其特征在于，在所述锆化处理之前对所述永磁体进行预处理；其中，所述预处理的步骤依次包括：①研磨；②脱脂；③第一次水洗；④酸洗除锈；⑤第二次水洗；⑥超声去灰。
  7. 如权利要求6所述的永磁体的表面处理方法，其特征在于，步骤①中，在所述研磨的过程中加入防锈剂；
    和/或，步骤①中，所述研磨在振动式研磨机中进行；
    和/或，步骤①中，所述研磨的温度为10-40℃；
    和/或，步骤①中，所述研磨的时间为2-36h；
    和/或，步骤②中，在所述脱脂的过程中加入除油粉；
    和/或，步骤②中，所述脱脂的温度为45-55℃；
    和/或，步骤②中，所述脱脂的时间为3-7min；
    和/或，步骤③中，所述第一次水洗分别在第一水洗槽和第二水洗槽中进行；
    和/或，步骤③中，所述第一次水洗的时间为10-20秒；
    和/或，步骤③中，所述第一次水洗的溢流水流量为100立方/小时；
    和/或，步骤④中，所述酸洗除锈的时间为30-50s；
    和/或，步骤④中，所述酸洗除锈的酸为稀硝酸；
    和/或，步骤⑤中，所述第二次水洗在第三水洗槽中进行；
    和/或，步骤⑤中，所述第二次水洗的时间为10-20秒；
    和/或，步骤⑤中，所述第二次水洗的溢流水流量为100立方/小时；
    和/或，步骤⑥中，所述超声去灰在第四水洗槽中进行；
    和/或，步骤⑥中，进行所述超声去灰前，加入超声保护剂；
    和/或，步骤⑥中，所述超声去灰的时间为2-5min。
  8. 如权利要求7所述的永磁体的表面处理方法，其特征在于，步骤①中，所述防锈剂包括磷酸钠、碳酸钠、氢氧化钠和OP-10乳化剂中的一种或多种；较佳地，所述磷酸钠的浓度为60-80g/L，碳酸钠40-60g/L，氢氧化钠5-10g/L或OP-10乳化剂0.05-1g/L中的一种或多种；
    和/或，步骤④中，所述稀硝酸的浓度为1％-3％；
    和/或，步骤⑥中，所述超声保护剂的浓度为0.1-1％，所述超声保护剂的浓度为超声保护剂占所述第四水洗槽的洗涤水的质量百分比。
  9. 一种永磁体，其特征在于，其采用如权利要求1-8任一项所述的永磁体的表面处理方法得到。
  10. 一种永磁体保护膜，其特征在于，其由如权利要求1-8任一项所述的永磁体的表面处理方法得到。
PCT/CN2023/090163 2022-10-25 2023-04-23 永磁体的表面处理方法、永磁体及其保护膜 WO2024087548A1 (zh)

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