CN114592223B - Neodymium-iron-boron magnet galvanization and surface lubrication process - Google Patents

Neodymium-iron-boron magnet galvanization and surface lubrication process Download PDF

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CN114592223B
CN114592223B CN202210290235.3A CN202210290235A CN114592223B CN 114592223 B CN114592223 B CN 114592223B CN 202210290235 A CN202210290235 A CN 202210290235A CN 114592223 B CN114592223 B CN 114592223B
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neodymium
iron
boron magnet
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galvanization
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CN114592223A (en
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邵江龙
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Sino Magnetics Technology Co Ltd
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Sino Magnetics Technology Co Ltd
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    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/34Pretreatment of metallic surfaces to be electroplated
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    • C10PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10MLUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M173/00Lubricating compositions containing more than 10% water
    • C10M173/02Lubricating compositions containing more than 10% water not containing mineral or fatty oils
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    • 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
    • C23C22/05Chemical 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
    • C23C22/06Chemical 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 aqueous acidic solutions with pH less than 6
    • C23C22/46Chemical 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 aqueous acidic solutions with pH less than 6 containing oxalates
    • C23C22/47Chemical 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 aqueous acidic solutions with pH less than 6 containing oxalates containing also phosphates
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    • 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
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    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/22Electroplating: Baths therefor from solutions of zinc
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    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48After-treatment of electroplated surfaces
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    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
    • C25D5/48After-treatment of electroplated surfaces
    • C25D5/52After-treatment of electroplated surfaces by brightening or burnishing
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    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D7/00Electroplating characterised by the article coated
    • C25D7/001Magnets
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01FMAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
    • H01F1/00Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties
    • H01F1/01Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials
    • H01F1/03Magnets or magnetic bodies characterised by the magnetic materials therefor; Selection of materials for their magnetic properties of inorganic materials characterised by their coercivity
    • H01F1/032Magnets 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
    • H01F1/04Magnets 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
    • H01F1/047Alloys characterised by their composition
    • H01F1/053Alloys characterised by their composition containing rare earth metals
    • H01F1/055Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5
    • H01F1/057Alloys characterised by their composition containing rare earth metals and magnetic transition metals, e.g. SmCo5 and IIIa elements, e.g. Nd2Fe14B
    • 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
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    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/06Metal compounds
    • C10M2201/062Oxides; Hydroxides; Carbonates or bicarbonates
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    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/085Phosphorus oxides, acids or salts
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    • C10M2201/00Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/10Compounds containing silicon
    • C10M2201/105Silica
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    • C10M2219/00Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/042Sulfate esters
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    • 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
    • C23C2222/00Aspects relating to chemical surface treatment of metallic material by reaction of the surface with a reactive medium
    • C23C2222/10Use of solutions containing trivalent chromium but free of hexavalent chromium

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Abstract

The invention provides a lubricating liquid for a surface of a neodymium-iron-boron galvanized magnet and a galvanization lubrication process, and relates to the technical field of neodymium-iron-boron galvanization. Specifically, the method comprises the following steps of S1 pretreatment before electroplating: sequentially carrying out acid washing, ultrasonic water washing and activation treatment on the neodymium-iron-boron magnet; s2, galvanization: electroplating the pretreated neodymium-iron-boron magnet at normal temperature, and forming a coating with the thickness of 6-8 mu m on the surface of the neodymium-iron-boron magnet; s3, electroplating post-treatment: sequentially carrying out light emitting and passivation treatment on the galvanized neodymium-iron-boron magnet, and forming a passivation film of 0.5-0.8 mu m on the surface of the neodymium-iron-boron magnet; s4 lubrication sealing: completely immersing the neodymium-iron-boron magnet in the lubricating liquid at the temperature of 40-60 ℃ for 10 seconds; s5, drying treatment. The preparation process is simple to operate and low in energy consumption, and the lubricating film layer can be added on the surface of the galvanized layer of the NdFeB magnet only by optimizing and adjusting process parameters and adding the lubricating liquid treatment step in the electroplating process, so that the performance requirements of galvanization, adhesion and lubrication are simultaneously met. Has the advantages of simple operation and simple process.

Description

Neodymium-iron-boron magnet galvanization and surface lubrication process
Technical Field
The invention belongs to the technical field of neodymium iron boron galvanization, and particularly relates to a neodymium iron boron magnet galvanization and surface lubrication process.
Background
In recent years, the application and development of neodymium iron boron (NdFeB) permanent magnetic materials are very rapid, and the materials are mainly prepared from rare earth neodymium Nd, iron, boron and other elements through a powder metallurgy process. As the strongest magnetic material at present, the magnetic material has been widely applied to the fields of electroplating devices, machinery, medical treatment, automobiles and the like, and has very broad application prospect.
With the development of production technology and the complex and changeable requirements of the application environment of the magnet in different industries, the requirements on the performance of the product are increased. By taking a galvanized product as an example, the surface of the neodymium iron boron magnet is galvanized in the past, but the surface is galvanized, the salt fog is usually needed to be 48-72 hours in the galvanization process, and the adhesive property is improved; in addition, in order to improve the sorting efficiency and prevent the damage of the plating layer caused by friction in the sheet selecting step, the surface of the zinc layer also needs a lubrication process. Therefore, the development of a simple production process flow capable of simultaneously meeting the requirements of galvanization, adhesion and lubrication of the neodymium-iron-boron magnet is a problem to be solved by the technicians in the field.
Disclosure of Invention
The invention aims to provide a zinc plating and surface lubrication process for a neodymium-iron-boron magnet, wherein a lubrication film layer can be added on the surface of a zinc plating layer of the neodymium-iron-boron magnet only by optimizing and adjusting process parameters and adding a lubrication liquid treatment step in the electroplating process, so that the performance requirements of zinc plating, mucilage glue and lubrication are met. Has the advantages of simple operation and simple process.
In order to achieve the above purpose, the invention provides a process for galvanization and surface lubrication of a neodymium iron boron magnet, which specifically comprises the following steps:
s1 pretreatment before electroplating: sequentially carrying out acid washing, ultrasonic water washing and activation treatment on the neodymium-iron-boron magnet;
s2, galvanization: completely immersing the pretreated neodymium-iron-boron magnet in a galvanization solution with the pH value of 4.6-5.0, and electroplating at normal temperature to form a plating layer with the thickness of 6-8 mu m on the surface of the neodymium-iron-boron magnet;
s3, electroplating post-treatment: sequentially carrying out light emitting and passivation treatment on the galvanized neodymium-iron-boron magnet, and forming a passivation film of 0.5-0.8 mu m on the surface of the neodymium-iron-boron magnet;
s4 lubrication sealing: completely immersing the neodymium-iron-boron magnet subjected to light emission and passivation treatment in a lubricating liquid, treating for 10 seconds at 50 ℃, and forming a lubricating film of 0.5-0.8 mu m on the surface of the neodymium-iron-boron magnet;
s5, drying: and wiping the NdFeB magnet after the lubrication treatment, and drying to finish the galvanization and surface lubrication process.
In a preferred embodiment, in step S1, the pickling operation is: the neodymium-iron-boron magnet is completely immersed in the pickling solution for 20-30 seconds, wherein the pickling solution is nitric acid with the volume fraction of 2%.
In a preferred embodiment, in step S1, the ultrasonic water washing operation is as follows: and washing the acid-washed neodymium-iron-boron magnet with water for 60 seconds at normal temperature under the ultrasonic condition.
In a preferred embodiment, in step S1, the activating operation is: completely immersing the neodymium-iron-boron magnet subjected to ultrasonic water washing in an activating solution for 4-6 seconds, wherein the activating solution is hydrochloric acid with the volume fraction of 2%; after activation, the activated product can be washed with flowing water for 2-4 times.
According to the invention, through three steps of acid washing, ultrasonic washing and activation in the pretreatment before S1 electroplating, dust and impurities on the surface of the neodymium-iron-boron magnet can be removed, and the electroplating effect is prevented from being influenced by mixing impurities in the electroplating process. Wherein, because the surface of the neodymium ferromagnetic product is provided with an oxide film, the oxide film can be removed by acid washing, otherwise, the electroplated layer has poor binding force or peeling; boron ash still remains on the surface after pickling, so that the boron ash is removed by ultrasonic cleaning; the activation before plating has the following functions: the surface of the product is uniformly corroded again, so that the surface roughness of the product is increased, and the combination of the coating and the matrix is firmer.
In a preferred embodiment, in step S2, the zinc plating solution includes: 200-240g/L of potassium chloride, 30-40g/L of zinc chloride, 30-50g/L of boric acid, water as solvent, 4.6-5.0 of galvanization pH and 0.5-2A/dm of cathode current density 2 The galvanization time is 65 minutes; more preferably, the zinc plating solution includes: 220g/L of potassium chloride, 35g/L of zinc chloride and 40g/L of boric acid.
In the invention, the electroplating solution component selects 35g/L of zinc chloride, which is different from other potassium chloride galvanization processes, and aims at low zinc content, and the formed electroplated layer is compact and wear-resistant. If the PH of the electroplating solution is less than 4.6, plating is slow, a formed matrix is easy to corrode, and the binding force of a plating layer is poor. Moreover, a large number of experiments prove that the compactness, the wear resistance and the binding force of the plating layer formed by the plating solution PH within the range of 4.6-5.0 are obviously better than those of other ranges, and the sealing film and the zinc layer can be combined more firmly when the plating solution is used for passivation and subsequent lubrication sealing treatment.
In a preferred embodiment, in step S3, the light emitting operation is as follows: the electroplated neodymium-iron-boron magnet is completely immersed in the light-emitting liquid for 5-10 seconds, wherein the light-emitting liquid is nitric acid with the volume fraction of 0.5%, and the neodymium-iron-boron magnet can be cleaned for 15 seconds by flowing water after light-emitting treatment.
In the invention, the effect of light emission is to remove the fog layer on the surface of the plating layer, and the zinc layer is brighter.
In a preferred embodiment, in step S3, the passivation operation is: immersing the neodymium-iron-boron magnet subjected to light-emitting treatment in trivalent color passivation solution;
the trivalent color passivation solution comprises the following components in parts by weight: 2.5-3 parts of chromium nitrate, 0.5-1 part of cobalt nitrate, 0.1-0.2 part of sodium hydroxide, 0.2-0.3 part of oxalic acid, 0.1-0.2 part of phosphoric acid, 2.5-3 parts of complexing agent and 90-95 parts of water, wherein the trivalent color passivation solution comprises 100 parts of components; passivating the pH value of the passivating solution at 2.1-2.8 at 30-40 ℃ for 40-50 seconds;
in the invention, zinc complex is mainly formed on the surface of the zinc layer by passivation, and the salt fog effect of the zinc complex is increased by more than 20 times compared with that of pure zinc plating. The trivalent color passivation solution is mainly passivation solution which does not contain hexavalent chromium, and hexavalent chromium belongs to serious harmful substances and is controlled in an environment-friendly key way. The invention is characterized in that the trivalent passivation film layer reacts with the A, B type sealing liquid in the step S4 to form the sealing film, the color of the passivation film is not changed, and the sealing film and the passivation film act together to support the protection of a matrix, thereby simultaneously meeting the performance requirements of galvanization, viscose and lubrication.
In a preferred embodiment, in step S4, the pH value of the lubricating fluid is 8-10, and the volume ratio of the type a sealing fluid to the type B sealing fluid is 1:1, mixing to obtain the product;
the A-type sealing liquid comprises the following components in parts by weight: 1-8 parts of Lugalvan DC, 2-7 parts of silicon dioxide, 0.5-1 part of 30% concentration lithium polysilicate solution, 84-98 parts of water, and 100 parts of A-type sealing liquid;
the B-type sealing liquid comprises the following components in parts by weight: 1.8-7.2 parts of sodium dodecyl sulfate, 0.6-2.4 parts of trisodium phosphate, 0.12 parts of sodium hydroxide and 90-98 parts of water, wherein the B-type sealing liquid comprises 100 parts of components.
In the invention, the A-type sealing liquid mainly acts on the organic film layer on the surface of the product to improve the salt spray of the product, the B-type sealing liquid mainly enhances the lubricity of the product, and the combination of A and B aims at not only not reducing the salt spray effect of the passivation film, but also improving the lubricity of the product. However, if the stock solutions A and B are used directly, precipitates are formed, so that the lubricating effect must be ensured by mixing the stock solutions A and B in the specific ratio before use. The pH of the sealing liquid is adjusted to 8-10 in order to reduce corrosion of the passivation film.
The AB type sealing liquid raw material essence used in the invention is simple and easy to purchase, the cost is low, and in order to further reduce the use cost, the used sealing liquid can be recovered and filtered to remove impurities, and then the A and B stock solutions are added according to the original proportion for continuous use. Practical experiments prove that the sealing liquid which is recycled and filtered is not obviously changed in salt fog, binding force and lubricating property after being recycled for 100 times, so that the sealing liquid can be fully recycled, and the production cost is further reduced.
More preferably, in step S4, the type a sealing solution includes the following components in parts by weight: 4 parts of Lugalvan DC, 4 parts of silicon dioxide, 0.6 part of a lithium polysilicate solution with the concentration of 30 percent and 91.4 parts of water; the B-type sealing liquid comprises the following components in parts by weight: 4.5 parts of sodium dodecyl sulfate, 1.5 parts of trisodium phosphate, 0.12 part of sodium hydroxide and 93.88 parts of water.
In a preferred embodiment, in step S5, the drying temperature is 70 ℃ and the drying time is 30 minutes.
Another object of the present invention is to provide a neodymium iron boron magnet prepared according to the above galvanization and surface lubrication processes.
Compared with the prior art, the plating zinc and surface lubrication process for the neodymium iron boron magnet has the following advantages:
1. the galvanization and surface lubrication process designed in the invention has simple operation, low energy consumption and easy control of the production process, and can increase the lubrication film layer on the surface of the galvanized layer of the NdFeB magnet only by optimizing and adjusting parameters and increasing the treatment step of the lubrication liquid in the electroplating process, thereby simultaneously meeting the performance requirements of galvanization, adhesion and lubrication. Has the advantages of simple operation and simple process.
2. The lubricating liquid used by the invention has simple components, low cost and easy acquisition, and can greatly reduce the production cost on the premise of keeping good lubricating effect. The used sealing liquid can be recovered and filtered, and the stock solutions A and B can be added according to the original ratio for continuous use, so that the production cost can be further reduced on the premise of keeping the sealing performance unchanged.
3. The neodymium iron magnet galvanized product prepared by the process can meet the industry standard by practical detection of salt fog and adhesive force; during the subsequent sorting and ring pasting operation, the product has good lubricating performance and smooth surface, and even the magnetized strong magnetic products can be efficiently separated, thereby achieving the purpose of improving the production efficiency. Through actual measurement and calculation, the sorting and ring pasting efficiency is improved by more than 30% compared with the traditional process.
Detailed Description
Unless otherwise indicated, the technical means used in the examples are conventional means well known to those skilled in the art, and all raw materials used are commercially available.
Unless otherwise specifically indicated, various raw materials, reagents, instruments, equipment, etc. used in the present invention are commercially available or can be prepared by existing methods, wherein the complexing agent model is OXAC-304B20, brand name: schuldada, germany, available from dehn chemical company, inc; lugalvan DC brand: basf, available from de En chemical Co., ltd; lithium polysilicate solutions were purchased from de En chemical Co.
In the present invention, the parts by weight may be those known in the art such as mu g, mg, g, kg, or may be multiples thereof such as 1/10, 1/100, 10 times, 100 times, etc.
The test criteria of the present invention are as follows,
salt mist: the NdFeB products prepared by different processes are prepared into a size of 30.75.2.3 mm, and a neutral salt spray test scheme of national standard of GB6458-86 salt spray test is adopted;
tackiness: preparing NdFeB products prepared by different processes into a size of 30.75.2.3 mm, using 603 anaerobic adhesive to be adhered on a tool, standing for 48 hours at normal temperature, and using a universal tester to perform pressure test;
lubricity: average number C of neodymium iron magnetic products separated by 100 staff within 8 hours of counting 1 Average number C of non-galvanized neodymium ferromagnetic products separated by the same staff within 8 hours of counting 0 Lubricating effect increase rate= (C 1 -C 0 )/C 0 *100%。
Example 1:
s1 pretreatment before electroplating: firstly, carrying out acid washing treatment on the neodymium-iron-boron magnet: completely immersing the neodymium-iron-boron magnet in 2% nitric acid for 30 seconds; then washing the acid-washed neodymium-iron-boron magnet for 60 seconds at normal temperature under the ultrasonic condition; finally, completely immersing the neodymium-iron-boron magnet subjected to ultrasonic water washing in hydrochloric acid with the volume fraction of 2% for 5 seconds; after activation, the mixture can be washed with flowing water for 2 times.
S2, galvanization: completely immersing the pretreated neodymium-iron-boron magnet in a zinc plating solution with the pH value of 4.6-5.0, and electroplating at normal temperature, wherein the zinc plating solution comprises: 220g/L of potassium chloride, 35g/L of zinc chloride, 40g/L of boric acid, water as solvent and 0.5-2A/dm of cathode current density 2 The galvanizing time is 55-65 minutes, and a plating layer of 6-8 mu m is formed on the surface of the NdFeB magnet after the galvanizing.
S3, electroplating post-treatment: completely immersing the galvanized neodymium-iron-boron magnet in nitric acid with the volume fraction of 0.5% for 5 seconds to carry out light-emitting treatment, and cleaning the neodymium-iron-boron magnet with flowing water for 15 seconds after the light-emitting treatment;
then, immersing the neodymium-iron-boron magnet subjected to light-emitting treatment into trivalent color zinc passivation solution, and finally forming a passivation film of 0.5-0.8 mu m on the surface of the neodymium-iron-boron magnet;
wherein, when trivalent color zinc is handled, the passivation solution includes: 3 parts of trivalent chromium salt (chromium nitrate), 0.8 part of cobalt nitrate, 0.2 part of sodium hydroxide, 0.2 part of oxalic acid, 0.2 part of phosphoric acid, 3 parts of complexing agent OXAC-304B20 (a product of XYZ, germany), 93 parts of water, 2.6 parts of pH value of passivation solution and passivation for 45 seconds at 30 ℃.
S4 lubrication sealing: completely immersing the neodymium-iron-boron magnet subjected to light emission and passivation treatment in a lubricating liquid, and treating for 10 seconds at 50 ℃; forming a lubricating film of 0.5-0.8 mu m on the surface of the NdFeB magnet;
the pH value of the lubricating liquid is 8.6, and the lubricating liquid is prepared from A-type sealing liquid and B-type sealing liquid according to the volume ratio of 1:1, wherein the A-type sealing liquid comprises the following components in parts by weight: 4 parts of Lugalvan DC, 4 parts of silicon dioxide, 0.6 part of a lithium polysilicate solution with the concentration of 30 percent and 91.4 parts of water; the B-type sealing liquid comprises the following components in parts by weight: 4.5 parts of sodium dodecyl sulfate, 1.5 parts of trisodium phosphate, 0.12 part of sodium hydroxide and 93.88 parts of water.
S5, drying: and drying the NdFeB magnet subjected to the wiping lubrication treatment at 60-70 ℃ for 20-30 minutes to finish the galvanization and surface lubrication processes.
Example 2
In the step S4, the used lubricating liquid is with the pH value of 8.6, and the volume ratio of the A-type sealing liquid to the B-type sealing liquid is 1:1, wherein the A-type sealing liquid is prepared by mixing, by weight, 3 parts of Lugalvan DC, 3 parts of silicon dioxide, 0.5 part of a lithium polysilicate solution with the concentration of 30%, and 93.5 parts of water; the B-type sealing liquid comprises the following components in parts by weight: 3.5 parts of sodium dodecyl sulfate, 1 part of trisodium phosphate, 0.1 part of sodium hydroxide and 95.4 parts of water.
The remaining steps and starting materials were the same as in example 1.
Comparative example 1
In the step S4, the lubricating liquid is only A-type sealing liquid, and comprises the following components in parts by weight: 4 parts of Lugalvan DC, 4 parts of silicon dioxide, 0.6 part of a lithium polysilicate solution with the concentration of 30 percent and 91.4 parts of water.
The remaining steps and starting materials were the same as in example 1.
Comparative example 2
In the step S4, the lubricating liquid is only B-type sealing liquid, and comprises the following components in parts by weight: 4.5 parts of sodium dodecyl sulfate, 1.5 parts of trisodium phosphate, 0.12 part of sodium hydroxide and 93.88 parts of water.
The remaining steps and starting materials were the same as in example 1.
Comparative example 3
In the technical solution of embodiment 1, step S4, i.e. direct drying after the completion of the S3 plating post-treatment, is omitted.
The remaining steps and starting materials were the same as in example 1.
Effect example
The neodymium ferromagnetic materials treated by the galvanization lubrication process of examples 1-2 and comparative examples 1-2 were tested for salt spray, adhesion and lubricity, and the results are shown in table 1.
Table 1 data of salt spray, tackiness, lubricity were measured for neodymium ferromagnetic materials treated by different galvanization lubrication processes.
The foregoing descriptions of specific exemplary embodiments of the present invention are presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain the specific principles of the invention and its practical application to thereby enable one skilled in the art to make and utilize the invention in various exemplary embodiments and with various modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.

Claims (4)

1. The process for galvanization and surface lubrication of the neodymium-iron-boron magnet is characterized by comprising the following steps of:
s1 pretreatment before electroplating: sequentially carrying out acid washing, ultrasonic water washing and activation treatment on the neodymium-iron-boron magnet;
s2, galvanization: completely immersing the pretreated neodymium-iron-boron magnet in a galvanization solution with the pH value of 4.6-5.0, and electroplating at normal temperature to form a plating layer with the thickness of 6-8 mu m on the surface of the neodymium-iron-boron magnet;
s3, electroplating post-treatment: sequentially carrying out light emitting and passivation treatment on the galvanized neodymium-iron-boron magnet, and forming a passivation film of 0.5-0.8 mu m on the surface of the neodymium-iron-boron magnet;
s4 lubrication sealing: completely immersing the neodymium-iron-boron magnet subjected to light emission and passivation treatment in a lubricating liquid, treating for 10 seconds at the temperature of 40-60 ℃, and forming a lubricating film of 0.5-0.8 mu m on the surface of the neodymium-iron-boron magnet;
s5, drying: wiping the lubricated neodymium-iron-boron magnet, and drying to finish the galvanization and surface lubrication process;
in step S1, the pickling operation is as follows: completely immersing the neodymium-iron-boron magnet in pickling solution for 20-30 seconds, wherein the pickling solution is nitric acid with the volume fraction of 2%;
the activation operation is as follows: completely immersing the neodymium-iron-boron magnet subjected to ultrasonic water washing in an activating solution for 4-6 seconds, wherein the activating solution is hydrochloric acid with the volume fraction of 2%; washing with flowing water for 2-4 times after activation;
in step S2, the zinc plating solution includes: 200-240g/L of potassium chloride, 30-40g/L of zinc chloride and 30-50g/L of boric acid, and the cathode current density is 0.5-2A/dm 2 The galvanization time is 55-65 minutes;
in step S3, the light emitting operation is: completely immersing the electroplated neodymium-iron-boron magnet in a light-emitting liquid for 5-10 seconds, wherein the light-emitting liquid is nitric acid with the volume fraction of 0.5%, and washing the neodymium-iron-boron magnet for 15 seconds by flowing water after light-emitting treatment;
in step S3, the passivation operation is: immersing the neodymium-iron-boron magnet subjected to light-emitting treatment in trivalent color passivation solution; the trivalent color passivation solution comprises the following components in parts by weight: 2.5-3 parts of chromium nitrate, 0.5-1 part of cobalt nitrate, 0.1-0.2 part of sodium hydroxide, 0.2-0.3 part of oxalic acid, 0.1-0.2 part of phosphoric acid, 2.5-3 parts of complexing agent and 90-95 parts of water, wherein the trivalent color passivation solution comprises 100 parts of components;
passivating the pH value of the passivating solution at 2.1-2.8 at 30-40 ℃ for 40-50 seconds;
in the step S4, the pH value of the lubricating liquid is 8-10, and the volume ratio of the A-type sealing liquid to the B-type sealing liquid is 1:1, mixing to obtain the product;
the A-type sealing liquid comprises the following components in parts by weight: 1-8 parts of Lugalvan DC, 2-7 parts of silicon dioxide, 0.5-1 part of 30% concentration lithium polysilicate solution, 84-98 parts of water, and 100 parts of A-type sealing liquid;
the B-type sealing liquid comprises the following components in parts by weight: 1.8-7.2 parts of sodium dodecyl sulfate, 0.6-2.4 parts of trisodium phosphate, 0.12 parts of sodium hydroxide and 90-98 parts of water, wherein the B-type sealing liquid comprises 100 parts of components.
2. The process for galvanization and surface lubrication of a neodymium iron boron magnet according to claim 1, wherein in step S1, the ultrasonic washing operation is: and washing the acid-washed neodymium-iron-boron magnet with water for 60 seconds at normal temperature under the ultrasonic condition.
3. The process for galvanizing a neodymium iron boron magnet and lubricating the surface of the neodymium iron boron magnet according to claim 1, wherein in the step S5, the drying temperature is 70 ℃, and the drying time is 30 minutes.
4. The neodymium-iron-boron magnet prepared by the surface lubrication process according to claim 1.
CN202210290235.3A 2022-03-23 2022-03-23 Neodymium-iron-boron magnet galvanization and surface lubrication process Active CN114592223B (en)

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