CN114481113A - Post-processing method and application of neodymium iron boron phosphide magnet - Google Patents

Post-processing method and application of neodymium iron boron phosphide magnet Download PDF

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Publication number
CN114481113A
CN114481113A CN202210032837.9A CN202210032837A CN114481113A CN 114481113 A CN114481113 A CN 114481113A CN 202210032837 A CN202210032837 A CN 202210032837A CN 114481113 A CN114481113 A CN 114481113A
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CN
China
Prior art keywords
magnet
drying
iron boron
neodymium iron
post
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Pending
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CN202210032837.9A
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Chinese (zh)
Inventor
时宗华
刘明辉
曹林峰
赵占中
陈静武
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Earth Bear Baotou Permanent Magnet Technology Co ltd
Earth Panda Advance Magnetic Material Co Ltd
Original Assignee
Earth Bear Baotou Permanent Magnet Technology Co ltd
Earth Panda Advance Magnetic Material Co Ltd
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Priority to CN202210032837.9A priority Critical patent/CN114481113A/en
Publication of CN114481113A publication Critical patent/CN114481113A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23CCOATING 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
    • C23C22/00Chemical 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
    • C23C22/82After-treatment
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F41/00Apparatus 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
    • H01F41/02Apparatus 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
    • H01F41/0253Apparatus 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
    • H01F41/026Apparatus 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

Abstract

The invention discloses a post-processing method and application of a phosphorized neodymium-iron-boron magnet, which mainly comprise the following steps: phosphorizing the neodymium iron boron magnet to obtain a phosphorized neodymium iron boron magnet; washing the neodymium iron boron phosphide magnet; and (3) placing the washed neodymium iron boron phosphide magnet in inert gas for drying. The post-treatment method can finish drying the phosphated neodymium iron boron magnet in a relatively static state, has short drying time and low energy consumption, and obviously improves the corrosion resistance of the dried neodymium iron boron magnet.

Description

Post-processing method and application of neodymium iron boron phosphide magnet
Technical Field
The invention belongs to the technical field of surface treatment of neodymium iron boron magnets, and particularly relates to a post-treatment method of a phosphated neodymium iron boron magnet, and further relates to application of the post-treatment method in preparation of the neodymium iron boron magnet.
Background
Neodymium iron boron is widely used in various fields such as aerospace, medical treatment, military and the like as a magnetic material. Neodymium iron boron is a multi-element powder alloy material, is very easy to oxidize due to addition of various rare earth elements in the production process, is generally subjected to surface treatment in order to prevent magnet oxidation and prolong the service life of the magnet, and various surface treatment methods such as electroplating, spraying, phosphating and the like are widely applied to the field.
The phosphorization is used as a conventional surface treatment method for the neodymium iron boron magnet, and has the advantages of low cost, simple operation and poor corrosion resistance, is usually only used for short-time corrosion resistance, solves the problem that the magnet is not oxidized in the packaging and transportation processes, and improves the corrosion resistance by spraying paint, injection molding and other methods.
Due to the characteristics of easy oxidation of the magnet and poor corrosion resistance of the phosphating film, the magnet is influenced by temperature and oxygen in the drying process after phosphating, so that the neodymium-iron-boron magnet after phosphating has poor corrosion resistance and is easy to rust, the drying process is carried out manually in small batches in many times, and the proportion of unqualified rusting is reduced by shortening the drying time; as shown in fig. 1, after washing with water, the magnet is dried by hot air, and in addition, during the drying process, the magnet needs to be continuously turned over to achieve the purpose of uniform heating, but during the turning over process, mutual friction easily has a negative effect on the compactness of the phosphating film.
Disclosure of Invention
In view of the above, the present invention needs to provide a post-treatment method for a phosphated ndfeb magnet, wherein the phosphated ndfeb magnet can be dried in a relatively static state, the drying time is short, the energy consumption is low, and the corrosion resistance of the dried ndfeb magnet is significantly improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a post-processing method of a phosphorized neodymium-iron-boron magnet, which comprises the following steps:
phosphorizing the neodymium iron boron magnet to obtain a phosphorized neodymium iron boron magnet;
washing the neodymium iron boron phosphide magnet;
and (3) placing the washed neodymium iron boron phosphide magnet in inert gas for drying.
In a further scheme, the drying step specifically comprises:
introducing inert gas into the drying equipment to evacuate air in the drying equipment, and filling the drying equipment with the inert gas;
and placing the washed neodymium-iron-boron magnet into the drying equipment for drying.
In a further scheme, in the drying process, the drying equipment is filled with the inert gas all the time.
In a further scheme, the drying temperature is 60-90 ℃, and the drying time is 3-8 min.
Further, the inert gas is selected from group 0 noble gases or nitrogen.
The invention further provides the use of a post-treatment method as defined in any one of the preceding claims in the preparation of a neodymium iron boron magnet.
Compared with the prior art, the invention has the following beneficial effects:
the post-treatment method can be used for drying the phosphated neodymium-iron-boron magnet in a relatively static state, is simple to operate, short in drying time and low in drying temperature, and can reduce energy consumption in the post-treatment process. Most importantly, the corrosion resistance of the neodymium iron boron magnet dried by the post-treatment method is obviously improved.
The post-processing method can improve the production efficiency and the rate of certified products.
Drawings
FIG. 1 is a process flow of the post-treatment of a prior phosphated neodymium-iron-boron magnet;
fig. 2 is a process flow of post-treatment of the phosphated ndfeb magnet in a preferred embodiment of the present invention.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the specific embodiments illustrated. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The first aspect of the present invention provides a post-processing method for a neodymium iron boron phosphide magnet, as shown in fig. 2, comprising the following steps:
phosphorizing the neodymium iron boron magnet to obtain a phosphorized neodymium iron boron magnet;
washing the neodymium iron boron phosphide magnet;
and (3) placing the washed neodymium iron boron phosphide magnet in inert gas for drying.
On the basis of the original process, the washed neodymium iron boron phosphide is dried in an inert atmosphere, so that on one hand, the operation is simple, the drying time is short, and the energy consumption can be remarkably reduced; on the other hand, after drying, the corrosion resistance of the phosphatized neodymium iron boron can be obviously improved, and the rate of certified products of the neodymium iron boron magnet is improved.
It is understood that the phosphating, water washing and the like described herein are all conventional processes for producing neodymium iron boron in the art, and are not particularly limited, and thus are not specifically described herein.
According to an embodiment of the present invention, the drying step specifically includes: introducing inert gas into the drying equipment to evacuate air in the drying equipment, and filling the drying equipment with the inert gas; placing the washed neodymium-iron-boron magnet in drying equipment for drying; preferably, the drying apparatus is filled with the inert gas at all times during the drying. It is understood that the drying apparatus is not particularly limited, and may be performed on the basis of an existing drying apparatus, and it should be noted that sufficient sealing performance is ensured, and in addition, the inert gas in the drying apparatus may be monitored, and if the threshold requirement is not met, the inert gas may be supplemented in time, so as to ensure that the drying apparatus is filled with the inert gas all the time in the whole drying process. Compared with the traditional hot air drying mode, the drying mode has better drying effect, does not need to continuously turn over the magnet, and can quickly dry in a short time under the relatively static condition; compared with vacuum drying, the conventional sintering furnace consumes more than 30min when vacuumized to 0.1Pa, so that the time consumption is long, the heating process consumes more time, the energy consumption is high, and the efficiency is low.
According to the embodiment of the invention, the drying temperature is 60-90 ℃ and the drying time is 3-8 min.
The inert gas described herein is not particularly limited, and is selected from group 0 noble gases (e.g., helium, argon, etc.) or nitrogen.
The second aspect of the invention provides an application of the post-treatment method in preparation of the neodymium iron boron magnet, and the corrosion resistance of the neodymium iron boron magnet can be effectively improved by introducing the post-treatment method in any neodymium iron boron preparation process.
The present invention is illustrated below by way of specific examples, which are intended to be illustrative only and not to limit the scope of the present invention in any way, and reagents and materials used therein are commercially available, unless otherwise specified, and conditions or steps thereof are not specifically described.
The test items in the following examples and comparative examples are specifically as follows:
damp heat test: the temperature is 85 +/-3 ℃ and the humidity is 100 percent RH;
saline soak experiment: 3% sodium chloride solution;
and (3) appearance detection: and (4) visual inspection.
Comparative example 1
Taking 5kg of neodymium iron boron magnet, phosphorizing at 35 ℃ for 15min, washing with water for 2min, and drying the phosphorized neodymium iron boron magnet for 5min by adopting hot air of a blower, wherein the drying temperature is 75 ℃, and the neodymium iron boron magnet is continuously turned over in the drying process.
The dried ndfeb magnets were randomly taken and subjected to a damp heat test, a brine soaking test and an appearance test, respectively, with the results shown in tables 1 and 2.
TABLE 1 Damp-Heat test and salt Water soak test results
Categories Quantity (tablet) 10h 12h 15h
Damp-heat test 10 Has no change Has no change 4 pieces rust
Immersion test 10 Has no change Has no change Rust on the whole
TABLE 2 appearance test results of 200 pieces of magnet
Categories Quantity (tablet) Slight corrosion (sheet) Fraction defective Percent of pass
Visual inspection 200 2 1% 99%
Example 1
The same embodiment as in comparative example 1 was used except that: and (3) drying the washed neodymium iron boron phosphide in a drying device filled with nitrogen for 5min at the drying temperature of 75 ℃.
The dried ndfeb magnets were randomly taken and subjected to a damp heat test, a brine soaking test and an appearance test, respectively, with the results shown in tables 3 and 4.
TABLE 3 Damp-Heat test and salt Water soak test results
Categories Quantity (tablet) 10h 12h 15h
Damp-heat test 10 Has no change Has no change Without change
Immersion test 10 Has no change Without change Has no change
TABLE 4 appearance test results of 200 pieces of magnet in full test
Categories Quantity (tablet) Slight corrosion (sheet) Fraction defective Percent of pass
Visual inspection 200 0 0 100%
Example 2
The same embodiment as in comparative example 1 was used except that: and (3) drying the washed neodymium iron boron phosphide in drying equipment filled with helium for 8min at the drying temperature of 60 ℃.
Example 3
The same embodiment as in comparative example 1 was used except that: and (3) drying the washed neodymium iron boron phosphide in a drying device filled with argon for 3min at the drying temperature of 90 ℃.
The same wet heat and brine soaking experiments as those in example 1 were performed on the neodymium iron boron magnet dried in example 2 and example 3, and the results are the same as those in example 1, and after the neodymium iron boron magnet was soaked in wet heat for 15 hours and brine for 15 hours, the neodymium iron boron magnet was not changed, and the qualified rate of the magnet appearance was 100%.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.

Claims (6)

1. The post-treatment method of the phosphorized neodymium-iron-boron magnet is characterized by comprising the following steps:
phosphorizing the neodymium iron boron magnet to obtain a phosphorized neodymium iron boron magnet;
washing the neodymium iron boron phosphide magnet;
and (3) drying the washed neodymium iron boron phosphide magnet in inert gas.
2. The post-treatment method according to claim 1, characterized in that the drying step is in particular:
introducing inert gas into the drying equipment to evacuate air in the drying equipment, and filling the drying equipment with the inert gas;
and placing the washed neodymium-iron-boron magnet into the drying equipment for drying.
3. The post-treatment method according to claim 2, wherein the drying apparatus is filled with the inert gas at all times during the drying.
4. The post-treatment process according to claim 1, characterized in that the drying temperature is between 60 ℃ and 90 ℃ and the time is between 3 and 8 min.
5. The post-treatment method according to claim 1, wherein the inert gas is selected from group 0 noble gases or nitrogen.
6. Use of the post-treatment method according to any one of claims 1 to 5 for the preparation of neodymium iron boron magnets.
CN202210032837.9A 2022-01-12 2022-01-12 Post-processing method and application of neodymium iron boron phosphide magnet Pending CN114481113A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102732871A (en) * 2011-04-15 2012-10-17 中国科学院金属研究所 Neodymium iron boron magnet material phosphating treatment and organic coating double layers protection method
CN102936455A (en) * 2012-10-31 2013-02-20 沈阳中北通磁科技股份有限公司 Neodymium iron boron rare earth permanent magnet surface anti-corrosion coating and preparation method thereof
CN107723693A (en) * 2017-11-03 2018-02-23 安徽新合富力科技有限公司 A kind of Nd Fe B alloys method for bonderizing
CN109003799A (en) * 2018-07-06 2018-12-14 杭州永磁集团振泽磁业有限公司 A kind of preparation method of high-coercive force neodymium iron boron magnetic body
CN109504960A (en) * 2017-09-14 2019-03-22 天津市诚瑞丰科技有限公司 A kind of preprocess method of sheet metal component
CN111763936A (en) * 2020-07-07 2020-10-13 苏州市吴中区曙光铜管厂 Pre-passivation treatment process for inner wall of seamless smooth copper pipe

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102732871A (en) * 2011-04-15 2012-10-17 中国科学院金属研究所 Neodymium iron boron magnet material phosphating treatment and organic coating double layers protection method
CN102936455A (en) * 2012-10-31 2013-02-20 沈阳中北通磁科技股份有限公司 Neodymium iron boron rare earth permanent magnet surface anti-corrosion coating and preparation method thereof
CN109504960A (en) * 2017-09-14 2019-03-22 天津市诚瑞丰科技有限公司 A kind of preprocess method of sheet metal component
CN107723693A (en) * 2017-11-03 2018-02-23 安徽新合富力科技有限公司 A kind of Nd Fe B alloys method for bonderizing
CN109003799A (en) * 2018-07-06 2018-12-14 杭州永磁集团振泽磁业有限公司 A kind of preparation method of high-coercive force neodymium iron boron magnetic body
CN111763936A (en) * 2020-07-07 2020-10-13 苏州市吴中区曙光铜管厂 Pre-passivation treatment process for inner wall of seamless smooth copper pipe

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