CN107958759B - Rare earth permanent magnetic material with lasting wettability and surface treatment method for preparing material - Google Patents
Rare earth permanent magnetic material with lasting wettability and surface treatment method for preparing material Download PDFInfo
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- CN107958759B CN107958759B CN201610906529.9A CN201610906529A CN107958759B CN 107958759 B CN107958759 B CN 107958759B CN 201610906529 A CN201610906529 A CN 201610906529A CN 107958759 B CN107958759 B CN 107958759B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F1/00—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
- H01F1/01—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
- H01F1/03—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
- H01F1/032—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials
- H01F1/04—Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity of hard-magnetic materials metals or alloys
- H01F1/047—Alloys characterised by their composition
- H01F1/053—Alloys characterised by their composition containing rare earth metals
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- 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
- H01F41/0253—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 for manufacturing permanent magnets
- H01F41/026—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 for manufacturing permanent magnets protecting methods against environmental influences, e.g. oxygen, by surface treatment
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Abstract
The invention provides a rare earth permanent magnetic material with durable wettability and a surface treatment method required for preparing the rare earth permanent magnetic material by using a wetting agent. The surface of the rare earth permanent magnetic material provided by the invention is provided with a layer of organic film, and the organic film contains any one or more of urea, polypropylene glycol 200, polyethylene glycol 200, glycerol, sorbitol and propylene glycol. The technical scheme provided by the invention can effectively improve the wettability of the existing rare earth permanent magnet material, thereby solving various problems caused by poor wettability in the storage and use processes.
Description
Technical Field
The invention belongs to the field of rare earth permanent magnet materials, and particularly relates to a rare earth permanent magnet material and a surface treatment method for preparing the rare earth permanent magnet material.
Background
The rare earth permanent magnet material is easy to corrode and generally needs to be used after electroplating, and the degree of wetting of a coating by an adhesive is an important index for judging whether the rare earth permanent magnet material can be applied in the fields of automobiles, elevators and the like. Only if the surface of the plating layer has good wettability, the adhesive can be coated on the surface of the plating layer in a large area, and good bonding force is formed. Therefore, the rare earth permanent magnet material has good sealing performance in the use process, is not easy to fall off and is durable in use. Therefore, customers have high requirements on the wettability of the electroplated layer of the rare earth permanent magnet material.
The reduction of the wettability of the plating layer is mainly caused by pollution of the inspection process and the reduction of the surface tension of the plating layer due to dust adsorption on the surface of a product in the processes of storage and transportation. It is understood that most neodymium iron boron manufacturers currently, in order to meet the requirements of customers for wettability, are usually cleaned, i.e. degreased + activated, before shipping. Although the method can quickly recover the wettability of the rare earth permanent magnet material coating, the method not only increases the production cost (labor, oil removal and activation), but also causes potential quality risks such as knocking and bulging of the product in the cleaning process.
The rare earth permanent magnetic materials have various shapes, and the method for improving the wettability needs to have universality and meet the continuous production condition. And because the permanent magnet product needs to be stored for a certain time from the completion of electroplating to the final use, the improved wettability is required to be well maintained.
The prior art discloses several methods for improving wettability, but basically has the defects of complicated process, incapability of meeting the requirement of continuous production, toxic action even on central nerves and no description on the wettability retention time after improvement.
Disclosure of Invention
The invention mainly aims to provide a rare earth permanent magnet material with lasting wettability, and overcomes the defects of easy falling, low durability and the like possibly existing in the use process of the conventional rare earth permanent magnet material. It is another object of the present invention to provide a wetting agent that is effective in improving the wettability of rare earth permanent magnetic materials. It is another object of the present invention to provide a surface treatment method with simple process for improving the wettability of rare earth permanent magnetic material.
According to one aspect of the invention, the invention provides a rare earth permanent magnet material with durable wettability, wherein the surface of the rare earth permanent magnet material is provided with a layer of organic film, and the organic film contains any one or more of urea, polypropylene glycol 200, polyethylene glycol 200, glycerol, sorbitol and propylene glycol.
In one embodiment of the present invention, the organic film has a thickness of 0.1 to 1 μm.
According to another aspect of the present invention, the present invention further provides a wetting agent for processing a rare earth permanent magnetic material, the wetting agent comprises a film forming agent and water, the film forming agent comprises one or more of urea, polypropylene glycol 200, polyethylene glycol 200, glycerol, sorbitol and propylene glycol, and the content of the film forming agent is 40-200 ml/l.
In one embodiment of the invention, the film forming agent is present in an amount of 80-120 ml/l.
In one embodiment of the invention, the wetting agent further comprises a film aid agent, the film aid agent comprises one or more of polypropylene glycol 2000-8000 and polyethylene glycol 2000-8000, and the content of the film aid agent is 20-150 g/L.
In one embodiment of the present invention, the film aid is one or more of polypropylene glycol 6000, polyethylene glycol 2000 and polyethylene glycol 4000.
In one embodiment of the invention, the wetting agent further comprises a tension agent, the tension agent comprises one or more of secondary alkyl sodium sulfonate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate, and the content of the surfactant is 0.1-1 g/L.
According to another aspect of the present invention, the present invention also provides a surface treatment method for preparing the above rare earth permanent magnetic material, the surface treatment method comprising the steps of:
electroplating: electroplating the rare earth permanent magnet material which is formed after mechanical processing;
soaking: soaking the electroplated rare earth permanent magnet material in the wetting agent;
drying: and drying the soaked rare earth permanent magnet material.
In one embodiment of the present invention, the temperature of the soaking step is set to 15 to 60 ℃, and the soaking time is set to 10 to 120 seconds.
In one embodiment of the present invention, the temperature of the drying step is set to 80 to 120 ℃, and the drying time is set to 5 to 25 minutes.
The rare earth permanent magnetic material provided by the invention has good wettability, and the wettability is still good in a long time.
The wetting agent provided by the invention has a simple formula, and can effectively improve the wettability of the rare earth permanent magnet material. In addition, the wetting agent provided by the invention is environment-friendly and pollution-free, and can be used for a long time.
The surface treatment method provided by the invention has the advantages that the electroplated rare earth permanent magnet material is directly placed in the wetting agent for soaking, and then is dried, so that the process is simple. Moreover, the soaking time is very short, the requirements on equipment are low, and the required investment is low. Therefore, the surface treatment method provided by the invention is simple and rapid, and meets the requirement of continuous production. In addition, the surface treatment method provided by the invention has no requirement on the shape of the rare earth permanent magnet material, and can be used for treating the rare earth permanent magnet materials in various shapes, so that the surface treatment method has great advantages for the rare earth permanent magnet material with a complex shape.
Drawings
FIG. 1 is a schematic view of a surface treatment process for preparing a permanent-magnetic rare-earth material with durable wettability.
Fig. 2 is a photograph of a portion of the rare earth permanent magnetic material prepared by an embodiment of the present invention after being placed for 60 days and subjected to # 38 wetting tension detection.
FIG. 3 is a photograph of a 38# wetting tension test performed on a portion of a rare earth permanent magnetic material prepared according to a comparative example of the present invention after being left for 60 days.
Fig. 4 is a photograph of a portion of the rare earth permanent magnetic material prepared by an embodiment of the present invention after being placed for 60 days and subjected to a 38# wetting tension test.
FIG. 5 is a photograph of a 38# wetting tension test performed on a portion of a rare earth permanent magnetic material prepared according to a comparative example of the present invention after being left for 60 days.
Fig. 6 is a photograph of a portion of the rare earth permanent magnetic material prepared by an embodiment of the present invention after being placed for 60 days and subjected to # 38 wetting tension detection.
FIG. 7 is a photograph of a 38# wetting tension test performed on a portion of a rare earth permanent magnetic material prepared according to a comparative example of the present invention after being left for 60 days.
Fig. 8 is a photograph of a portion of the rare earth permanent magnetic material prepared by an embodiment of the present invention after being placed for 60 days and subjected to # 38 wetting tension detection.
FIG. 9 is a photograph of a 38# wetting tension test performed on a portion of a rare earth permanent magnetic material prepared according to a comparative example of the present invention after being left for 60 days.
Fig. 10 is a photograph of a portion of the rare earth permanent magnetic material prepared by an embodiment of the present invention after being placed for 60 days and then being subjected to a 38# wetting tension test.
FIG. 11 is a photograph of a 38# wetting tension test performed on a portion of a rare earth permanent magnetic material prepared according to a comparative example of the present invention after being left for 60 days.
Fig. 12 is a photograph of a portion of the rare earth permanent magnetic material prepared by an embodiment of the present invention after being placed for 60 days and then being subjected to a 38# wetting tension test.
FIG. 13 is a photograph of a 38# wetting tension test performed on a portion of a rare earth permanent magnetic material prepared according to a comparative example of the present invention after being left for 60 days.
Detailed Description
The following detailed description of the present invention, taken in conjunction with the accompanying drawings and examples, is provided to enable the invention and its various aspects and advantages to be better understood. However, the specific embodiments and examples described below are for illustrative purposes only and are not limiting of the invention.
It is to be noted that, in the present invention, 200, 6000, 2000 and 4000 out of polypropylene glycol 200, polyethylene glycol 200, polypropylene glycol 6000, polyethylene glycol 2000 and polyethylene glycol 4000 refer to average molecular weights of these substances; in addition, polypropylene glycol 2000-8000 and polyethylene glycol 2000-8000 refer to polypropylene glycol and polyethylene glycol having an average molecular weight of 2000-8000.
The surface of the rare earth permanent magnet material provided by the invention is adhered with a layer of organic film, and the organic film contains any one or more of urea, polypropylene glycol 200, polyethylene glycol 200, glycerol, sorbitol and propylene glycol.
The surface tension of urea, polypropylene glycol 200, polyethylene glycol 200, glycerin, sorbitol and propylene glycol is small, spreading can be completed on the surface of the electroplated layer of the rare earth permanent magnet material, and pollution to the electroplated layer in the inspection and storage processes is well prevented; and because the permanent magnetic material needs to be bonded by epoxy resin glue in actual use, an organic film formed by the substances has good affinity with the epoxy resin glue, so that the epoxy resin glue can well wet the surface of an electroplated layer to finish the bonding process. Therefore, the invention introduces the chemicals into the rare earth permanent magnet material industry for the first time so as to solve the problem of poor wetting of the current rare earth permanent magnet material.
A large number of experiments prove that the rare earth permanent magnetic material provided by the invention has very good wettability and can keep the good wettability for a long time.
The thinner the thickness of the organic film, the better the thickness of the organic film, so as not to affect the subsequent use of the rare earth permanent magnetic material, and preferably, the thickness of the organic film is 0.1 to 1 μm.
The main raw materials of the wetting agent provided by the invention are any one or more of urea, polypropylene glycol 200, polyethylene glycol 200, glycerin, sorbitol and propylene glycol, and the chemicals are called film forming agents in the invention. The content of film forming agent in the wetting agent is 40-200 ml/l, so that the wettability of the rare earth permanent magnetic material can be effectively improved. Through a large number of experiments, it was found that the optimum content of film formers in the wetting agent was 80-120 ml/l.
In order to improve the bonding strength of the film layer, some film aid agent can be added into the wetting agent. A large number of experiments show that the polypropylene glycol and the polyethylene glycol with the molecular weight of 2000-8000 can effectively improve the bonding strength of the film-forming agent and the electroplated layer, wherein the polypropylene glycol 6000, the polyethylene glycol 2000 or the polyethylene glycol 4000 have the best effect. The polypropylene glycol 2000-8000 and the polyethylene glycol 2000-8000 can be used alone or in combination, and are not particularly limited and can be determined according to actual needs.
A large number of experiments show that when the content of film forming agents in the wetting agent is 40-200 ml/L, the content of polypropylene glycol 2000-8000 and polyethylene glycol 2000-8000 in the wetting agent exceeds 20 g/L, and if the dosage exceeds 150 g/L, the solution viscosity is too high, so that the surface of the treated product is flowered and the organic film is not favorable for uniform thickness.
In order to reduce the surface tension of the wetting agent, the film forming agent is easy to form a film on the electroplated coating of the rare earth permanent magnet material, and the wetting agent can also be added with the tension agent. Through a large number of experiments, secondary sodium alkyl sulfonate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate can effectively improve the film forming property of urea, polypropylene glycol 200, polyethylene glycol 200, glycerol, sorbitol and propylene glycol on a plating layer. The secondary sodium alkylsulfonate, sodium dodecylsulfate and sodium dodecylbenzenesulfonate may be used alone or in combination, and are not particularly limited.
A large number of experiments show that the content of the film forming agent in the wetting agent is 40-200 ml/l, and the content of the tension agent in the wetting agent only needs to exceed 0.1 g/l. In addition, because the tension agent has strong foaming effect, if the dosage of the tension agent exceeds 1 g/L, the surface of the solution is filled with a large amount of foam, which is not beneficial to production operation and causes uneven surface color of the treated product.
In the present invention, the wetting agent may contain both the film aid and the tonicity agent, or may contain none or only one of them, in addition to the film forming agent.
As shown in fig. 1, on the basis of the above, the present invention further provides a surface treatment method for preparing the rare earth permanent magnetic material with durable wettability, which comprises three steps of electroplating, soaking and drying, specifically as follows:
electroplating: electroplating the rare earth permanent magnet material which is formed after mechanical processing.
The specific electroplating mode is not particularly limited and depends on the application and the process requirement of the rare earth permanent magnet material.
Soaking: the electroplated rare earth permanent magnet material is soaked in the above-mentioned wetting agent.
The time for soaking is not particularly limited, but in order to improve the production efficiency, when the temperature is set to 15 to 60 ℃ during soaking, it takes only 10 to 120 seconds to sufficiently adhere the wetting agent to the rare earth permanent magnet material. If the temperature is too low or too high, the wetting agent is difficult to adhere to the rare earth permanent magnet material, and the time required for soaking is prolonged; in particular, since most of the wetting agents provided by the present invention are surfactants, temperatures that are too high may not be effective.
Drying: and drying the soaked rare earth permanent magnet material.
The drying temperature and time are not particularly limited, the drying temperature is low, and the drying time is correspondingly prolonged; the temperature is high, the drying time is correspondingly short, however, the wetting agent can start to volatilize due to the high temperature, so that the film on the surface of the rare earth permanent magnet material is reduced, and the wettability of the rare earth permanent magnet material is affected. A large number of experiments show that the optimal drying temperature is 80-120 ℃, and the optimal drying time is 5-25 minutes.
The surface treatment method provided by the invention does not have any requirement on equipment as long as the process conditions can be met.
The present invention will be described below with reference to specific examples. The process condition values taken in the following examples are exemplary and can take values in the ranges set forth in the foregoing summary. The detection methods used in the following examples are all conventional in the industry.
Example 1
The raw material used in this example is a machined rare earth permanent magnet material with a specification of D23.8 × 2.5 mm. The mechanical processing means is chamfering, a vibration finishing machine is adopted for chamfering, 50kg of brown corundum abrasive is used for grinding for 8 hours. After chamfering, 30 g/L of sodium hydroxide solution and 2 g/L of OP-10 emulsifier (commercially available) are used as cleaning solution, and under the conditions of frequency of 20KHZ, power of 2KW and temperature of 40 ℃, the chamfered rare earth permanent magnet material is put into an ultrasonic cleaning machine for degreasing for 3 minutes. After oil removal, the mixture is pickled by 5 percent nitric acid at normal temperature for 40 seconds and then is put into an ultrasonic cleaning machine filled with clear water for cleaning.
The surface treatment method used in this example is shown in fig. 1, and specifically includes the following steps:
the electroplating step adopts processes of nickel plating, copper plating and semi-bright nickel plating.
Wherein, the nickel plating process conditions are as follows: 250 g/L of nickel sulfate, 30 g/L of nickel chloride and 35 g/L of boric acid, the temperature is 45 ℃, the PH value is 4.5, the plating solution is continuously filtered, and the plating time is 80 minutes;
copper plating process conditions are as follows: 60 g/l of copper pyrophosphate, 250 g/l of potassium pyrophosphate, pyrophosphate: copper ion ═ 7.0: 1, continuously filtering the plating solution at the temperature of 40 ℃ and the pH value of 8.2, and carrying out electroplating for 40 minutes;
the technological conditions of the semi-bright nickel are as follows: 250 g/L of nickel sulfate, 30 g/L of nickel chloride, 35 g/L of boric acid, 6 ml/L of semi-bright nickel additive, 45 ℃ of temperature, 4.5 of PH, continuous filtration of plating solution and 100 minutes of plating time.
The soaking step adopts the following process conditions:
sodium lauryl sulfate 0.3 g/l, urea 40 ml/l, propylene glycol 40 ml/l and polypropylene glycol 6000: 40 g/l, temperature 20 ℃, soaking treatment time: for 30 seconds.
The process conditions of the drying step are as follows:
the temperature was 120 ℃ for 10 minutes.
In this example, 50 pieces of rare earth permanent magnetic materials are prepared, and the 50 pieces of rare earth permanent magnetic materials are subjected to # 38 wetting tension detection at different times, and the detection results are shown in table 1. Fig. 2 is a photograph of a part of the rare earth permanent magnetic material after being placed for 60 days and subjected to # 38 wetting tension detection.
Comparative example 1
The comparative example used the same raw materials as in example 1, and the surface treatment method used was only electroplating, without the soaking and drying steps. The specific process conditions for electroplating were also the same as in example 1.
In the comparative example, 50 pieces of rare earth permanent magnetic materials are prepared, and the 50 pieces of rare earth permanent magnetic materials are subjected to 38# wetting tension detection at different times, and the detection results are shown in table 1. Fig. 3 is a photograph of a part of the rare earth permanent magnetic material after being placed for 60 days and subjected to # 38 wetting tension detection.
Example 2
The raw material used in this example is a machined rare earth permanent magnet material, and its specification is D17.9 × 3 mm. The mechanical processing means is chamfering, a vibration finishing machine is adopted for chamfering, 50kg of brown corundum abrasive is used for grinding for 14 hours. After chamfering, 30 g/L of sodium hydroxide solution and 2 g/L of OP-10 emulsifier (commercially available) are used as cleaning solution, and under the conditions of frequency of 20KHZ, power of 2KW and temperature of 40 ℃, the chamfered rare earth permanent magnet material is put into an ultrasonic cleaning machine for degreasing for 3 minutes. After oil removal, the mixture is pickled by 5 percent nitric acid at normal temperature for 40 seconds and then is put into an ultrasonic cleaning machine filled with clear water for cleaning.
The surface treatment method used in this example is shown in fig. 1, and specifically includes the following steps:
the electroplating step adopts processes of nickel plating, copper plating and semi-bright nickel plating.
Wherein, the nickel plating process conditions are as follows: 300 g/L of nickel sulfate, 50 g/L of nickel chloride and 50 g/L of boric acid, the temperature is 55 ℃, the PH value is 5.2, the plating solution is continuously filtered, and the plating time is 90 minutes;
copper plating process conditions are as follows: copper pyrophosphate 90 g/l, potassium pyrophosphate 350 g/l, pyrophosphate: copper ion ═ 8.0: 1, continuously filtering the plating solution at the temperature of 50 ℃ and the pH value of 8.8, and carrying out electroplating for 60 minutes;
the technological conditions of the semi-bright nickel are as follows: 300 g/L of nickel sulfate, 50 g/L of nickel chloride, 50 g/L of boric acid, 6 ml/L of semi-bright nickel additive, 55 ℃ of temperature, 5.2 of PH, continuous filtration of plating solution and 100 minutes of plating time.
The soaking step adopts the following process conditions:
sodium lauryl sulfate 0.6 g/l, urea 40 ml/l, sorbitol 60 ml/l, propylene glycol 60 ml/l and polypropylene glycol 6000: 80 g/l, temperature 30 ℃, soaking treatment time: for 20 seconds.
The process conditions of the drying step are as follows:
the temperature was 120 ℃ for 10 minutes.
In this example, 50 pieces of rare earth permanent magnetic materials are prepared, and the 50 pieces of rare earth permanent magnetic materials are subjected to # 38 wetting tension detection at different times, and the detection results are shown in table 2. Fig. 4 is a photograph of a part of the rare earth permanent magnetic material after being placed for 60 days and subjected to # 38 wetting tension detection.
Comparative example 2
The comparative example used the same raw materials as in example 2, and the surface treatment method used was only electroplating, without the soaking and drying steps. The specific process conditions for electroplating were also the same as in example 2.
In the comparative example, 50 pieces of rare earth permanent magnetic materials are prepared, and the 50 pieces of rare earth permanent magnetic materials are subjected to 38# wetting tension detection at different times, and the detection results are shown in table 2. Fig. 5 is a photograph of a part of the rare earth permanent magnetic material after being placed for 60 days and subjected to # 38 wetting tension detection.
Example 3
The raw material used in this example is a machined rare earth permanent magnet material, and its specification is D15.2 × 2 mm. The mechanical processing means is chamfering, a vibration finishing machine is adopted for chamfering, 50kg of brown corundum abrasive is used for grinding for 16 hours. After chamfering, 30 g/L of sodium hydroxide solution and 2 g/L of OP-10 emulsifier (commercially available) are used as cleaning solution, and under the conditions of frequency of 20KHZ, power of 2KW and temperature of 40 ℃, the chamfered rare earth permanent magnet material is put into an ultrasonic cleaning machine for degreasing for 3 minutes. After oil removal, the mixture is pickled by 5 percent nitric acid at normal temperature for 40 seconds and then is put into an ultrasonic cleaning machine filled with clear water for cleaning.
The surface treatment method used in this example is shown in fig. 1, and specifically includes the following steps:
the electroplating step adopts processes of nickel plating, copper plating and semi-bright nickel plating.
Wherein, the nickel plating process conditions are as follows: 260 g/L of nickel sulfate, 35 g/L of nickel chloride and 37 g/L of boric acid, the temperature is 48 ℃, the PH value is 4.8, the plating solution is continuously filtered, and the plating time is 80 minutes;
copper plating process conditions are as follows: 75 g/l of copper pyrophosphate, 280 g/l of potassium pyrophosphate, pyrophosphate: copper ion 7.7: 1, continuously filtering the plating solution at the temperature of 48 ℃ and the pH value of 8.4, wherein the plating time is 70 minutes;
the technological conditions of the semi-bright nickel are as follows: 260 g/L of nickel sulfate, 35 g/L of nickel chloride, 37 g/L of boric acid, 6 ml/L of semi-bright nickel additive, 48 ℃ of temperature, 4.8 of PH, continuous filtration of plating solution and 90 minutes of plating time.
The soaking step adopts the following process conditions:
secondary sodium alkyl sulfonate 0.4 g/l, sodium dodecylbenzenesulfonate 0.6 g/l, polypropylene glycol 200: 200 ml/l, polyethylene glycol 2000: 150 g/l, temperature 60 ℃, soaking treatment time: for 10 seconds.
The process conditions of the drying step are as follows:
the temperature was 80 ℃ for 25 minutes.
In this example, 50 pieces of rare earth permanent magnetic materials are prepared, and the 50 pieces of rare earth permanent magnetic materials are subjected to # 38 wetting tension detection at different times, and the detection results are shown in table 3. Fig. 6 is a photograph of a part of the rare earth permanent magnetic material after being placed for 60 days and subjected to # 38 wetting tension detection.
Comparative example 3
The comparative example used the same raw materials as in example 3, and the surface treatment method used was only electroplating, without the soaking and drying steps. The specific process conditions for electroplating were also the same as in example 3.
In the comparative example, 50 pieces of rare earth permanent magnetic materials are prepared, and the 50 pieces of rare earth permanent magnetic materials are subjected to 38# wetting tension detection at different times, and the detection results are shown in table 3. Fig. 7 is a photograph of a part of the rare earth permanent magnetic material after being placed for 60 days and subjected to # 38 wetting tension detection.
Example 4
The raw material used in this example is a machined rare earth permanent magnet material with a specification of D31 × 7 mm. The mechanical processing means is chamfering, a vibration finishing machine is adopted for chamfering, 50kg of brown corundum abrasive is used for grinding for 10 hours. After chamfering, 30 g/L of sodium hydroxide solution and 2 g/L of OP-10 emulsifier (commercially available) are used as cleaning solution, and under the conditions of frequency of 20KHZ, power of 2KW and temperature of 40 ℃, the chamfered rare earth permanent magnet material is put into an ultrasonic cleaning machine for degreasing for 3 minutes. After oil removal, the mixture is pickled by 5 percent nitric acid at normal temperature for 40 seconds and then is put into an ultrasonic cleaning machine filled with clear water for cleaning.
The surface treatment method used in this example is shown in fig. 1, and specifically includes the following steps:
the electroplating step adopts processes of nickel plating, copper plating and semi-bright nickel plating.
Wherein, the nickel plating process conditions are as follows: 290 g/L of nickel sulfate, 45 g/L of nickel chloride and 40 g/L of boric acid, the temperature is 55 ℃, the PH value is 5.1, the plating solution is continuously filtered, and the plating time is 70 minutes;
copper plating process conditions are as follows: copper pyrophosphate 70 g/l, potassium pyrophosphate 330 g/l, pyrophosphate: copper ion 7.5: 1, continuously filtering the plating solution at the temperature of 50 ℃ and the pH value of 8.6, wherein the plating time is 70 minutes;
the technological conditions of the semi-bright nickel are as follows: 300 g/L of nickel sulfate, 45 g/L of nickel chloride, 40 g/L of boric acid, 6 ml/L of semi-bright nickel additive, 55 ℃ of temperature, 5.1 of PH, continuous filtration of plating solution and 80 minutes of plating time.
The soaking step adopts the following process conditions:
sodium dodecyl sulfate 0.1 g/l, polyethylene glycol 200: 40 ml/l, polyethylene glycol 4000: 20 g/l, temperature 15 ℃, soaking treatment time: for 120 seconds.
The process conditions of the drying step are as follows:
the temperature was 110 ℃ for 5 minutes.
In this example, 50 pieces of rare earth permanent magnetic materials are prepared, and the 50 pieces of rare earth permanent magnetic materials are subjected to # 38 wetting tension detection at different times, and the detection results are shown in table 4. Fig. 8 is a photograph of a part of the rare earth permanent magnetic material after being placed for 60 days and subjected to # 38 wetting tension detection.
Comparative example 4
The comparative example used the same raw materials as in example 4, and the surface treatment method used was only electroplating, without the soaking and drying steps. The specific process conditions for electroplating were also the same as in example 4.
In the comparative example, 50 pieces of rare earth permanent magnetic materials are prepared, and the 50 pieces of rare earth permanent magnetic materials are subjected to 38# wetting tension detection at different times, and the detection results are shown in table 4. Fig. 9 is a photograph of a part of the rare earth permanent magnetic material after being placed for 60 days and subjected to # 38 wetting tension detection.
Example 5
The raw material used in this example is a machined rare earth permanent magnet material, and its specification is D20.7 × 2.8 mm. The mechanical processing means is chamfering, a vibration finishing machine is adopted for chamfering, 50kg of brown corundum abrasive is used for grinding for 13 hours. After chamfering, 30 g/L of sodium hydroxide solution and 2 g/L of OP-10 emulsifier (commercially available) are used as cleaning solution, and under the conditions of frequency of 20KHZ, power of 2KW and temperature of 40 ℃, the chamfered rare earth permanent magnet material is put into an ultrasonic cleaning machine for degreasing for 3 minutes. After oil removal, the mixture is pickled by 5 percent nitric acid at normal temperature for 40 seconds and then is put into an ultrasonic cleaning machine filled with clear water for cleaning.
The surface treatment method used in this example is shown in fig. 1, and specifically includes the following steps:
the electroplating step adopts processes of nickel plating, copper plating and semi-bright nickel plating.
Wherein, the nickel plating process conditions are as follows: 280 g/L of nickel sulfate, 40 g/L of nickel chloride and 45 g/L of boric acid, the temperature is 50 ℃, the PH value is 4.9, the plating solution is continuously filtered, and the plating time is 70 minutes;
copper plating process conditions are as follows: copper pyrophosphate 80 g/l, potassium pyrophosphate 300 g/l, pyrophosphate: copper ion ═ 8.0: 1, continuously filtering the plating solution at the temperature of 45 ℃ and the pH value of 8.6, wherein the plating time is 80 minutes;
the technological conditions of the semi-bright nickel are as follows: 270 g/L of nickel sulfate, 40 g/L of nickel chloride, 45 g/L of boric acid, 6 ml/L of semi-bright nickel additive, 50 ℃ of temperature, 4.9 of PH, continuous filtration of plating solution and 90 minutes of plating time.
The soaking step adopts the following process conditions:
sodium dodecyl benzene sulfonate 0.8 g/l, glycerin 120 ml/l, sorbitol: 40 ml/l, polypropylene glycol 4000: 120 g/l, temperature 50 ℃, soaking treatment time: for 80 seconds.
The process conditions of the drying step are as follows:
the temperature is 110 ℃ and the time is 15 minutes.
In this example, 50 pieces of rare earth permanent magnetic materials are prepared, and the 50 pieces of rare earth permanent magnetic materials are subjected to # 38 wetting tension detection at different times, and the detection results are shown in table 5. Fig. 10 is a photograph of a part of the rare earth permanent magnetic material after being placed for 60 days and subjected to # 38 wetting tension detection.
Comparative example 5
The comparative example used the same raw materials as in example 5, and the surface treatment method used was only electroplating, without the soaking and drying steps. The specific process conditions for electroplating were also the same as in example 5.
In the comparative example, 50 pieces of rare earth permanent magnetic materials are prepared, and the 50 pieces of rare earth permanent magnetic materials are subjected to 38# wetting tension detection at different times, and the detection results are shown in table 5. Fig. 11 is a photograph of a part of the rare earth permanent magnetic material after being placed for 60 days and subjected to # 38 wetting tension detection.
Example 6
The raw material used in this example is a machined rare earth permanent magnet material with a specification of 25 × 12 mm. The mechanical processing means is chamfering, the chamfering adopts a vibration finishing machine, 40kg of brown corundum abrasive material is used, and the vibration grinding is carried out for 8 hours. After chamfering, 30 g/L of sodium hydroxide solution and 2 g/L of OP-10 emulsifier (commercially available) are used as cleaning solution, and under the conditions of frequency of 20KHZ, power of 2KW and temperature of 40 ℃, the chamfered rare earth permanent magnet material is put into an ultrasonic cleaning machine for degreasing for 3 minutes. After oil removal, the mixture is pickled by 5 percent nitric acid at normal temperature for 40 seconds and then is put into an ultrasonic cleaning machine filled with clear water for cleaning.
The surface treatment method used in this example is shown in fig. 1, and specifically includes the following steps:
the electroplating step adopts a process of galvanizing.
Wherein, the galvanizing process conditions are as follows: 230 g/L of potassium chloride, 60 g/L of zinc chloride, 35 g/L of boric acid, 16 ml/L of zinc plating additive, room temperature, PH 6, continuous filtration of plating solution and 80 minutes of plating time.
The soaking step adopts the following process conditions:
sodium dodecylbenzenesulfonate 0.5 g/l, glycerin 100 ml/l, sorbitol: 60 ml/l, polypropylene glycol 4000: 70 g/l, temperature 50 ℃, soaking treatment time: for 70 seconds.
The process conditions of the drying step are as follows:
the temperature is 110 ℃ and the time is 15 minutes.
In this example, 50 pieces of rare earth permanent magnetic materials are prepared, and the 50 pieces of rare earth permanent magnetic materials are subjected to # 38 wetting tension detection at different times, and the detection results are shown in table 6. Fig. 12 is a photograph of a part of the rare earth permanent magnetic material after being placed for 60 days and subjected to # 38 wetting tension detection.
Comparative example 6
The comparative example used the same raw materials as in example 6, and the surface treatment method used was only electroplating, without the soaking and drying steps. The specific process conditions for electroplating were also the same as in example 6. In the comparative example, 50 pieces of rare earth permanent magnetic materials are prepared, and the 50 pieces of rare earth permanent magnetic materials are subjected to 38# wetting tension detection at different times, and the detection results are shown in table 6. Fig. 13 is a photograph of a part of the rare earth permanent magnetic material after being placed for 60 days and subjected to # 38 wetting tension detection.
Table 1 test results of example 1 and comparative example 1
Table 2 test results of example 2 and comparative example 2
Table 3 test results of example 3 and comparative example 3
Table 4 test results of example 4 and comparative example 4
Table 5 test results of example 5 and comparative example 5
Table 6 test results of example 6 and comparative example 6
As can be seen from fig. 2, fig. 4, fig. 6, fig. 8, fig. 10, and fig. 12, after the rare earth permanent magnetic materials prepared in examples 1 to 6 are subjected to # 38 wetting tension detection, the liquid is uniformly spread on the surface of the plating layer, which indicates that the wettability of the rare earth permanent magnetic material is good. Similarly, as can be seen from fig. 3, fig. 5, fig. 7, fig. 9, fig. 11 and fig. 13, after the 38# wetting tension test, the liquid shrinks on the surface of the coating, that is, the rare earth permanent magnet materials prepared in comparative examples 1 to 6 have partial poor wettability, and cannot meet the requirement of subsequent use.
As can be seen from tables 1 to 6, all of the rare earth permanent magnetic materials prepared in examples 1 to 6 have very good wettability, and even after being left for 60 days, the wettability is still qualified, i.e., it is shown that the rare earth permanent magnetic material provided by the present invention has durable wettability. Similarly, it can be seen from tables 1 to 6 that the wettability of some finished products is deteriorated after the rare earth permanent magnet material is placed for a short time, which affects the qualification rate of the finished products; and with time, the wettability of the rare earth permanent magnetic material subjected to electroplating only becomes unstable.
In conclusion, the rare earth permanent magnetic material provided by the invention has good wettability, and the wettability is still good in a long time.
The wetting agent provided by the invention has a simple formula, and can effectively improve the wettability of the rare earth permanent magnet material. In addition, the wetting agent provided by the invention is environment-friendly and pollution-free, and can be used for a long time.
The surface treatment method provided by the invention has the advantages that the electroplated rare earth permanent magnet material is directly placed in the wetting agent for soaking, and then is dried, so that the process is simple. Moreover, the soaking time is very short, the requirements on equipment are low, and the required investment is low. Therefore, the surface treatment method provided by the invention is simple and rapid, and meets the requirement of continuous production. In addition, the surface treatment method provided by the invention has no requirement on the shape of the rare earth permanent magnet material, and can be used for treating the rare earth permanent magnet materials in various shapes, so that the surface treatment method has great advantages for the rare earth permanent magnet material with a complex shape.
It should be noted that the above-mentioned embodiments described with reference to the drawings are only intended to illustrate the present invention and not to limit the scope of the present invention, and it should be understood by those skilled in the art that modifications and equivalent substitutions can be made without departing from the spirit and scope of the present invention. Moreover, all or a portion of any embodiment may be utilized with all or a portion of any other embodiment, unless stated otherwise.
Claims (8)
1. The surface treatment method for preparing the rare earth permanent magnet material with the lasting wettability is characterized in that a layer of organic film is arranged on the surface of the rare earth permanent magnet material, and the organic film contains any one or more of urea, polypropylene glycol 200, polyethylene glycol 200, glycerol, sorbitol and propylene glycol;
the surface treatment method comprises the following steps:
electroplating: electroplating the rare earth permanent magnet material which is formed after mechanical processing;
soaking: soaking the electroplated rare earth permanent magnet material in a wetting agent;
drying: drying the soaked rare earth permanent magnet material;
the wetting agent comprises a film forming agent and water, wherein the film forming agent comprises one or more of urea, polypropylene glycol 200, polyethylene glycol 200, glycerin, sorbitol and propylene glycol, and the content of the film forming agent is 40-200 ml/L;
the wetting agent also comprises an auxiliary film agent, the auxiliary film agent comprises one or more of polypropylene glycol 2000-8000 and polyethylene glycol 2000-8000, and the content of the auxiliary film agent is 20-150 g/L.
2. The surface treatment method according to claim 1, wherein the content of the film-forming agent is 80 to 120 ml/l.
3. The surface treatment method according to claim 1, wherein the filming aid is one or more of polypropylene glycol 6000, polyethylene glycol 2000 and polyethylene glycol 4000.
4. The surface treatment method according to claim 1, wherein the wetting agent further comprises a tonicity agent, the tonicity agent comprises one or more of secondary sodium alkyl sulfonate, sodium dodecyl sulfate and sodium dodecyl benzene sulfonate, and the content of the tonicity agent is 0.1 to 1 g/l.
5. The surface treatment method according to claim 1, wherein the temperature of the soaking step is set to 15 to 60 ℃, and the soaking time is set to 10 to 120 seconds.
6. The surface treatment method according to claim 1, wherein the temperature of the drying step is set to 80 to 120 ℃, and the drying time is set to 5 to 25 minutes.
7. A rare earth permanent magnetic material having a permanent wettability obtained by the surface treatment method according to any one of claims 1 to 6.
8. The rare earth permanent magnetic material according to claim 7, wherein the thickness of the organic film is 0.1-1 μm.
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| CN103184051A (en) * | 2012-01-01 | 2013-07-03 | 天津三环乐喜新材料有限公司 | Antioxidant used for preparing sintered NdFeB (neodymium iron boron) permanent magnet material |
| CN203325624U (en) * | 2013-07-26 | 2013-12-04 | 宁波市鄞州区亿能磁业有限公司 | Novel neodymium iron boron magnet |
| CN104292486B (en) * | 2014-11-03 | 2017-07-14 | 杭州东方表面技术有限公司 | A kind of proposition wettability treatment solution and its application method |
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