CN114592223A - Neodymium iron boron magnet galvanizing and surface lubricating process - Google Patents

Neodymium iron boron magnet galvanizing and surface lubricating process Download PDF

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CN114592223A
CN114592223A CN202210290235.3A CN202210290235A CN114592223A CN 114592223 A CN114592223 A CN 114592223A CN 202210290235 A CN202210290235 A CN 202210290235A CN 114592223 A CN114592223 A CN 114592223A
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iron boron
parts
neodymium iron
boron magnet
magnet
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CN114592223B (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
    • C23C22/82After-treatment
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    • C25D3/00Electroplating: Baths therefor
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    • C25D3/22Electroplating: Baths therefor from solutions of zinc
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    • C25D5/00Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
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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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    • 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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    • C10M2201/105Silica
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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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    • C10M2229/00Organic macromolecular compounds containing atoms of elements not provided for in groups C10M2205/00, C10M2209/00, C10M2213/00, C10M2217/00, C10M2221/00 or C10M2225/00 as ingredients in lubricant compositions
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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 surface lubricating liquid for a neodymium iron boron galvanized magnet and a galvanizing lubricating process, and relates to the technical field of neodymium iron boron galvanizing. The method specifically comprises the steps of pretreatment before electroplating in S1: sequentially carrying out acid washing, ultrasonic washing and activating treatment on the neodymium iron boron magnet; s2 galvanization: electroplating the pretreated neodymium iron boron magnet at normal temperature to form a 6-8 mu m coating 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 to form 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; and S5 drying treatment. The preparation process is simple to operate and low in energy consumption, and a lubricating film layer can be added on the surface of the neodymium iron boron magnet galvanized layer only by optimizing and adjusting process parameters and adding a lubricating liquid treatment step in the electroplating process, so that the performance requirements of galvanizing, gluing and lubricating are met simultaneously. Has the effects of simple operation and simple process.

Description

Neodymium iron boron magnet galvanizing and surface lubricating process
Technical Field
The invention belongs to the technical field of neodymium iron boron galvanizing, and particularly relates to a neodymium iron boron magnet galvanizing and surface lubricating process.
Background
In recent years, neodymium iron boron (NdFeB) permanent magnet materials are applied and developed rapidly, and the materials are mainly prepared from elements such as rare earth metal Nd, iron, boron and the like through a powder metallurgy process. As the strongest magnetic material at present, the magnetic material is widely applied to the fields of electroplating devices, machinery, medical treatment, automobiles and the like, and has very wide application prospect.
With the development of production technology and the complex and varied requirements of magnet application environments in different industries, the requirements on product performance are higher and higher. By taking a galvanized product as an example, only the surface of the neodymium iron boron magnet needs to be galvanized in the past, but now the surface is galvanized, the galvanizing process usually needs salt spray for 48 to 72 hours, and the adhesive performance is also improved; in addition, in order to improve the sorting efficiency and prevent the damage of a coating caused by friction in the sheet selecting step, a lubricating process is needed on the surface of the zinc layer. Therefore, the development of a simple production process flow capable of simultaneously satisfying the requirements of zinc plating, adhesion and lubrication performance of the neodymium iron boron magnet is an urgent problem to be solved by those skilled in the art.
Disclosure of Invention
The invention aims to provide a neodymium iron boron magnet galvanizing and surface lubricating process, which can increase a lubricating film layer on the surface of a neodymium iron boron magnet galvanizing layer only by optimizing and adjusting process parameters and adding a lubricating liquid treatment step in an electroplating process, thereby meeting the performance requirements of galvanizing, gluing and lubricating at the same time. Has the effects of simple operation and simple process.
In order to achieve the purpose, the invention provides a neodymium iron boron magnet galvanizing and surface lubricating process, which specifically comprises the following steps:
s1 pretreatment before electroplating: sequentially carrying out acid washing, ultrasonic washing and activating treatment on the neodymium iron boron magnet;
s2 galvanization: completely immersing the pretreated neodymium iron boron magnet into a zinc plating solution with the pH value of 4.6-5.0, and plating at normal temperature to form a 6-8 mu m plating layer 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 to form 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 polished and passivated Nd-Fe-B magnet in a lubricating liquid, treating at 50 ℃ for 10 seconds, and forming a lubricating film of 0.5-0.8 mu m on the surface of the Nd-Fe-B magnet;
s5 drying treatment: and wiping the lubricated neodymium iron boron magnet, and drying to finish the galvanizing and surface lubricating processes.
In a preferred embodiment, in step S1, the pickling operation is: and completely immersing the neodymium-iron-boron magnet in an acid washing liquid for 20-30 seconds, wherein the acid washing liquid is nitric acid with the volume fraction of 2%.
In a preferred embodiment, in step S1, the ultrasonic water washing operation is: and (3) washing the acid-washed neodymium iron boron magnet 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 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.
In the invention, through three steps of acid washing, ultrasonic water washing and activation in pretreatment before S1 electroplating, dust and impurities on the surface of the neodymium iron boron magnet can be removed, and impurities are prevented from being mixed in the electroplating process to influence the electroplating effect. Because the surface of the neodymium ferromagnetic product has an oxide film, the oxide film can be removed by acid washing, otherwise, the electroplated layer has poor binding force or peeling; the surface still has boron ash after acid cleaning, so the boron ash is removed by ultrasonic cleaning; the pre-plating activation functions are as follows: the surface of the product is uniformly corroded again, so that the surface unevenness of the product is increased, and the plating layer and the substrate are combined more firmly.
In a preferred embodiment, in step S2, the zinc plating solution includes: 240g/L of potassium chloride 200-The zinc plating solution is water, the PH value of the zinc plating solution is 4.6-5.0, and the cathode current density is 0.5-2A/dm2The galvanizing 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 components of the electroplating solution are 35g/L of zinc chloride, which is different from other potassium chloride galvanizing processes, and aims to reduce the zinc content and form a compact and wear-resistant electroplated layer. If the pH value of the electroplating solution is less than 4.6, the plating speed is slow, the formed matrix is easy to corrode, and the binding force of the plating layer is poor. Moreover, a large number of experiments prove that the performance effects of coating compactness, wear resistance and bonding force formed by the plating solution with the PH value of 4.6-5.0 are obviously better than those of other ranges, and the sealing film and the zinc layer can be bonded 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: and (3) completely immersing the electroplated neodymium-iron-boron magnet in brightening liquid for 5-10 seconds, wherein the brightening 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 brightening treatment.
In the invention, the light-emitting function is to remove the fogging layer on the surface of the coating, 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 extraction 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 passivation solution at a pH value of 2.1-2.8 for 40-50 seconds at a temperature of 30-40 ℃;
in the invention, the passivation effect mainly forms a zinc complex on the surface of the zinc layer, and the salt spray 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 used, the passivation solution does not contain hexavalent chromium, and the hexavalent chromium belongs to serious harmful substances, so that the environmental protection is mainly controlled. The process is characterized in that the trivalent passivation film layer reacts with A, B type sealing liquid in the step S4 to form a sealing film, the color of the passivation film is not changed, and the sealing film and the passivation film jointly play a role in matrix protection, so that the performance requirements of zinc plating, adhesion and lubrication are met at the same time.
In a preferred embodiment, in step S4, the pH of the lubricating fluid is 8-10, and the ratio of the type a confining fluid to the type B confining fluid is 1: 1, mixing to obtain;
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% lithium polysilicate solution, 84-98 parts of water and 100 parts of A-type confining 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 part of sodium hydroxide, 90-98 parts of water and 100 parts of B-type sealing liquid.
In the invention, the A-type confining liquid mainly acts on the surface organic film layer of the product to improve the salt fog of the product, the B-type confining liquid mainly enhances the lubricity of the product, and the combination of the A and the B aims to improve the lubricity of the product without reducing the salt fog effect of the passivation film. However, since precipitates are formed when the stock solutions A and B are used as they are, they must be mixed in the above-mentioned specific ratio before use to ensure the lubricating effect. The pH value of the sealing liquid is adjusted to be 8-10, so that the corrosion of the passivation film is reduced.
The AB type sealing liquid raw material used in the invention is simple and easy to purchase, the cost is low, in order to further reduce the use cost, the used sealing liquid can be recovered to filter impurities, and the A and B raw liquids are replenished according to the original proportion for continuous use. Practical experiments prove that after the recycled and filtered sealing liquid is recycled and reused for 100 times, salt spray, binding force and lubricating property have no obvious change, which shows that the sealing liquid can be recycled completely to further reduce the production cost.
More preferably, in step S4, the a-type sealing liquid includes the following components in parts by weight: 4 parts of Lugalvan DC, 4 parts of silicon dioxide, 0.6 part of 30% lithium polysilicate solution 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 mentioned galvanization and surface lubrication process.
Compared with the prior art, the neodymium iron boron magnet galvanizing and surface lubricating process has the following advantages:
1. the galvanizing and surface lubricating process designed in the invention has the advantages of simple operation, low energy consumption and easy control of the production process, and only needs to optimize and adjust parameters and add the step of lubricating liquid treatment in the electroplating process, so that a lubricating film layer can be added on the surface of the galvanized layer of the neodymium iron boron magnet, thereby simultaneously meeting the performance requirements of galvanizing, gluing and lubricating. Has the effects of simple operation and simple process.
2. The lubricating liquid used in 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 to filter impurities, and the A and B stock solutions are replenished according to the original proportion for continuous use, so that the production cost can be further reduced on the premise of keeping the sealing performance unchanged.
3. Through actual detection, salt spray and adhesive force of the neodymium-iron-magnetic zinc-plated product prepared by the process can meet the industrial standard; during subsequent sorting and ring attaching operation, the products have good lubricating property and smooth surfaces, so that the magnetized strong magnetic products can be efficiently separated, and the aim of improving the production efficiency is fulfilled. Through actual measurement and calculation, the sorting and ring attaching efficiency is improved by more than 30% compared with that of the traditional process.
Detailed Description
Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art, and the raw materials used are commercially available.
Unless otherwise specifically stated, the various raw materials, reagents, instruments, equipment, etc. used in the present invention are commercially available or may be prepared by existing methods, wherein the complexing agent is OXAC-304B20, brand name: schluda, Germany, from Deen chemical Co., Ltd; the Lugalvan DC brand is: basf, available from de en chemical ltd; lithium polysilicate solutions were purchased from de en chemical ltd.
In the present invention, the parts by weight may be in the units of μ g, mg, g, kg, etc. known in the art, or may be multiples thereof, such as 1/10, 1/100, 10, 100, etc.
The test criteria for the present invention are as follows,
salt spray: preparing neodymium iron boron products prepared by different processes into a size of 30 × 13.75 × 2.3mm, and adopting a national standard neutral salt spray test scheme of GB6458-86 salt spray test;
tackiness: making the neodymium iron boron products prepared by different processes into 30 x 13.75 x 2.3mm, adhering the neodymium iron boron products on a tool by using 603 anaerobic adhesive, standing the tool for 48 hours at normal temperature, and performing pressure test by using a universal testing machine;
lubricity: average quantity C of neodymium-iron-magnetic products separated by 100 employees in 8 hours1Average quantity C of unbleached neodymium-iron-magnetic products separated by same staff within 8 hours of counting0The lubrication effect increase rate is (C)1-C0)/C0*100%。
Example 1:
s1 pretreatment before electroplating: firstly, carrying out acid pickling treatment on a neodymium iron boron magnet: completely immersing the neodymium iron boron magnet in nitric acid with the volume fraction of 2% 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 membrane may be washed with running water 2 times.
S2 galvanization: completely immersing the pretreated neodymium iron boron magnet into zinc plating solution with the pH value of 4.6-5.0, and plating 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 a solvent and 0.5-2A/dm of cathode current density2The galvanizing time is 55-65 minutes, and a 6-8 mu m plating layer is formed on the surface of the neodymium iron boron magnet after 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 bright dipping treatment, and cleaning the magnet for 15 seconds by using flowing water after the bright dipping treatment;
then, immersing the neodymium iron boron magnet after the light extraction treatment into a 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, during trivalent color zinc treatment, the passivation solution comprises: 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 (German Spirauda product), 93 parts of water, and passivating at 30 ℃ for 45 seconds, wherein the pH value of the passivating solution is 2.6.
S4 lubrication sealing: completely immersing the neodymium-iron-boron magnet subjected to the light extraction and passivation treatment in lubricating liquid, and treating at the temperature of 50 ℃ for 10 seconds; then forming a lubricating film of 0.5-0.8 mu m on the surface of the neodymium iron boron 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 confining liquid comprises the following components in parts by weight: 4 parts of Lugalvan DC, 4 parts of silicon dioxide, 0.6 part of 30% lithium polysilicate solution 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 treatment: and (3) wiping the lubricated neodymium iron boron magnet, and drying for 20-30 minutes at the temperature of 60-70 ℃ to finish the galvanizing and surface lubricating processes.
Example 2
In step S4, the lubricating fluid used has a pH of 8.6 and is a mixture of type a confining fluid and type B confining fluid at a volume ratio of 1: 1, wherein the A-type confining liquid is prepared by mixing 3 parts of Lugalvan DC, 3 parts of silicon dioxide, 0.5 part of 30% lithium polysilicate solution and 93.5 parts of water in parts by weight; 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 the raw materials used were the same as in example 1.
Comparative example 1
In the step S4, the used lubricating liquid is only A-type confining liquid and comprises the following components in parts by weight: 4 parts of Lugalvan DC, 4 parts of silicon dioxide, 0.6 part of 30% lithium polysilicate solution and 91.4 parts of water.
The remaining steps and the raw materials used were the same as in example 1.
Comparative example 2
In the step S4, the used lubricating liquid is only B-type confining 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 the raw materials used were the same as in example 1.
Comparative example 3
In the technical solution of the embodiment 1, the step S4 is omitted, i.e. the step S3 is directly dried after the plating post-treatment is completed.
The remaining steps and starting materials were the same as in example 1.
Examples of effects
The neodymium ferromagnetic materials treated by the galvanization lubrication process of examples 1-2 and comparative examples 1-2 were tested for salt spray, tackiness, and lubricity, and the results are shown in table 1.
Table 1 detection of salt spray, viscosity, and lubricity data for neodymium ferromagnetic materials treated by different galvanization lubrication processes.
Figure BDA0003561525530000081
The foregoing descriptions of specific exemplary embodiments of the present invention have been 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 certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and 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 (10)

1. A neodymium iron boron magnet galvanization and surface lubrication process is characterized by comprising the following steps:
s1 pretreatment before electroplating: sequentially carrying out acid washing, ultrasonic washing and activating treatment on the neodymium iron boron magnet;
s2 galvanization: completely immersing the pretreated neodymium iron boron magnet into a zinc plating solution with the pH value of 4.6-5.0, and plating at normal temperature to form a 6-8 mu m plating layer 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 to form 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 polished and passivated Nd-Fe-B magnet in a lubricating liquid, treating at 40-60 ℃ for 10 seconds, and forming a lubricating film of 0.5-0.8 mu m on the surface of the Nd-Fe-B magnet;
s5 drying treatment: and wiping the lubricated neodymium iron boron magnet, and drying to finish the galvanizing and surface lubricating processes.
2. The ndfeb magnet galvanization and surface lubrication process as claimed in claim 1, wherein in step S1, the pickling operation is: and completely immersing the neodymium-iron-boron magnet in an acid washing liquid for 20-30 seconds, wherein the acid washing liquid is nitric acid with the volume fraction of 2%.
3. The ndfeb magnet galvanization and surface lubrication process as claimed in claim 1, wherein in step S1, the ultrasonic water washing operation is: and (3) washing the acid-washed neodymium iron boron magnet for 60 seconds at normal temperature under the ultrasonic condition.
4. The ndfeb magnet galvanization and surface lubrication process as claimed in claim 1, wherein in step S1, the activation operation is: completely immersing the neodymium iron boron magnet subjected to ultrasonic 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.
5. The ndfeb magnet galvanizing and surface lubricating process according to claim 1, wherein in step S2, the galvanizing solution includes: 240g/L of potassium chloride 200-2The galvanizing time is 55-65 minutes.
6. The ndfeb magnet galvanization and surface lubrication process as claimed in claim 1, wherein in step S3, the light emitting operation is: and (3) completely immersing the electroplated neodymium-iron-boron magnet in brightening liquid for 5-10 seconds, wherein the brightening 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 brightening treatment.
7. The ndfeb magnet galvanization and surface lubrication process as claimed in claim 1, wherein in step S3, the passivation operation is: immersing the neodymium-iron-boron magnet subjected to light extraction 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;
the pH value of the passivation solution is 2.1-2.8, and the passivation is carried out for 40-50 seconds at the temperature of 30-40 ℃.
8. The neodymium-iron-boron magnet galvanizing and surface lubricating process as claimed in claim 1, wherein in the step S4, the pH value of the lubricating liquid is 8-10, and the ratio of the volume of the type a confining liquid to the volume of the type B confining liquid is 1: 1, mixing to obtain;
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% lithium polysilicate solution, 84-98 parts of water and 100 parts of A-type confining 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 part of sodium hydroxide, 90-98 parts of water and 100 parts of B-type sealing liquid.
9. The ndfeb magnet galvanization and surface lubrication process according to claim 1, wherein in step S5, the drying temperature is 70 ℃ and the drying time is 30 minutes.
10. A NdFeB magnet produced by the NdFeB magnet galvanization and surface lubrication process of claim 1.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114959673A (en) * 2022-06-21 2022-08-30 北京科技大学广州新材料研究院 Sintered Nd-Fe-B permanent magnet composite material and preparation method and application thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016093286A1 (en) * 2014-12-10 2016-06-16 新日鐵住金株式会社 Surface treatment agent for zinc-plated steel sheets
CN108276811A (en) * 2017-12-11 2018-07-13 安徽开林新材料股份有限公司 Aqueous zinc-plated sealer of one kind and preparation method thereof
CN109385653A (en) * 2018-10-18 2019-02-26 苏州吉之美表面处理材料有限公司 It is zinc-plated watersoluble closed dose a kind of and its preparation method and application
CN111321441A (en) * 2020-04-10 2020-06-23 中磁科技股份有限公司 Full-automatic neodymium iron boron galvanizing process
CN113846360A (en) * 2021-09-06 2021-12-28 广东致卓环保科技有限公司 Non-phosphorus and non-cyanogen zinc plating process for neodymium iron boron magnet

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2016093286A1 (en) * 2014-12-10 2016-06-16 新日鐵住金株式会社 Surface treatment agent for zinc-plated steel sheets
CN108276811A (en) * 2017-12-11 2018-07-13 安徽开林新材料股份有限公司 Aqueous zinc-plated sealer of one kind and preparation method thereof
CN109385653A (en) * 2018-10-18 2019-02-26 苏州吉之美表面处理材料有限公司 It is zinc-plated watersoluble closed dose a kind of and its preparation method and application
CN111321441A (en) * 2020-04-10 2020-06-23 中磁科技股份有限公司 Full-automatic neodymium iron boron galvanizing process
CN113846360A (en) * 2021-09-06 2021-12-28 广东致卓环保科技有限公司 Non-phosphorus and non-cyanogen zinc plating process for neodymium iron boron magnet

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
张蕾;景璀;: "钕铁硼永磁材料电镀锌镍合金工艺", 电子工艺技术, no. 04, pages 230 - 232 *
蒋建忠: "镀锌层三价铬钝化及钝化膜的封闭处理", 电镀与涂饰, vol. 32, no. 10, pages 43 - 46 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114959673A (en) * 2022-06-21 2022-08-30 北京科技大学广州新材料研究院 Sintered Nd-Fe-B permanent magnet composite material and preparation method and application thereof

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