CN111334830A - Method for solving dyne value of neodymium iron boron product - Google Patents
Method for solving dyne value of neodymium iron boron product Download PDFInfo
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- CN111334830A CN111334830A CN202010278008.XA CN202010278008A CN111334830A CN 111334830 A CN111334830 A CN 111334830A CN 202010278008 A CN202010278008 A CN 202010278008A CN 111334830 A CN111334830 A CN 111334830A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
- C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
- C25D5/14—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium two or more layers being of nickel or chromium, e.g. duplex or triplex layers
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/60—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using alkaline aqueous solutions with pH greater than 8
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/48—After-treatment of electroplated surfaces
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01F—MAGNETS; INDUCTANCES; TRANSFORMERS; SELECTION OF MATERIALS FOR THEIR MAGNETIC PROPERTIES
- H01F41/00—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties
- H01F41/02—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets
- H01F41/0253—Apparatus or processes specially adapted for manufacturing or assembling magnets, inductances or transformers; Apparatus or processes specially adapted for manufacturing materials characterised by their magnetic properties for manufacturing cores, coils, or magnets for manufacturing permanent magnets
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Abstract
The invention discloses a method for solving the dyne value of a neodymium iron boron product, which comprises the following steps: performing electronickelling treatment on the neodymium iron boron product to obtain an electronickelling neodymium iron boron product, wherein the electronickelling treatment comprises plating a bottom nickel layer, plating a copper layer on the bottom nickel layer, plating a semi-bright nickel layer on the copper layer and plating a bright nickel layer on the semi-bright nickel layer; carrying out primary secondary counter-current washing on the nickel-electroplated neodymium iron boron product; placing the neodymium iron boron product through first secondary counter current water washing in passivation solution and carrying out passivation treatment to the surface formation at the neodymium iron boron product of electronickelling has the passivation layer of certain thickness, wherein, the principal ingredients of passivation solution include: cationic surfactant, sodium molybdate, sodium silicate, sodium phosphate, sodium hydroxide and sodium carbonate; and carrying out secondary countercurrent washing and drying treatment. The method of the invention has simple operation and low cost, and the product dyne value can easily reach the standard.
Description
Technical Field
The invention relates to the technical field of nickel plating post-treatment of neodymium iron boron products, in particular to a method for solving the dyne value of the neodymium iron boron products.
Background
Neodymium iron boron magnetic materials, which are the latest result of the development of rare earth permanent magnetic materials, are called "maga" due to their excellent magnetic properties. The neodymium iron boron magnetic material has extremely high magnetic energy and coercive force, and the advantage of high energy density enables the neodymium iron boron permanent magnetic material to be widely applied in modern industry and electronic technology, thereby enabling miniaturization, light weight and thinning of instruments, electro-acoustic motors, magnetic separation and magnetization and other equipment to be possible.
Currently, the surface requirements for nickel-plated products are increasing. In the past, the nickel plating product can meet the requirements of customers as long as the salt mist, the thickness, the uniformity and the color of a nickel layer are consistent. The existing customers have new requirements, namely a dyne value, namely a dyne pen is used for detecting the surface tension value of a product, which is lower than the standard 30(N/m), and the surface is not easy to color or adhere or has the risk of degumming after adhesion. Therefore, in order to meet the requirement of the dyne value, the prior method is to intentionally roughen the surface of the product, prolong the activation time before electroplating, plate the nickel layer as dark as possible, but the method is labor-consuming, the dyne value is sometimes not ideal, and the method is frequently reworked and wastes manpower and material resources.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
The present invention is directed to a method for solving the dyne value of an ndfeb product, which can solve the above problems of the prior art.
In order to achieve the above object, the present invention provides a method for solving the dyne value of a neodymium iron boron product, comprising the following steps: performing electronickelling treatment on the neodymium iron boron product to obtain an electronickelling neodymium iron boron product, wherein the electronickelling treatment comprises plating a bottom nickel layer, plating a copper layer on the bottom nickel layer, plating a semi-bright nickel layer on the copper layer and plating a bright nickel layer on the semi-bright nickel layer; carrying out primary secondary counter-current washing on the nickel-electroplated neodymium iron boron product; placing the neodymium iron boron product through first secondary counter current water washing in passivation solution and carrying out passivation treatment to the surface formation at the neodymium iron boron product of electronickelling has the passivation layer of certain thickness, wherein, the principal ingredients of passivation solution include: cationic surfactant, sodium molybdate, sodium silicate, sodium phosphate, sodium hydroxide and sodium carbonate; and carrying out secondary countercurrent washing and drying treatment.
In an embodiment of the present invention, wherein, by weight percentage, water: cationic surfactant 1: 0.05; water: sodium molybdate 1: 0.4; water: sodium silicate 1: 0.35; water: sodium phosphate 1: 0.1; water: sodium hydroxide 1: 0.05; water: sodium carbonate 1: 0.1.
In one embodiment of the invention, the passivating solution has a pH of from 10 to 12.
In one embodiment of the present invention, the thickness of the passivation layer is 0.002-0.003 mm.
In one embodiment of the invention, the passivation is performed in a drum with a passivation time of 10min and a drum speed of 11 revolutions per minute.
In one embodiment of the present invention, the thickness of the bottom nickel layer, the thickness of the semi-bright nickel layer and the thickness of the bright nickel layer are all in the range of 0.004-0.006 mm, and the thickness of the copper plating layer is in the range of 0.003-0.005 mm.
In one embodiment of the present invention, activation treatment and secondary recovery are required before and after the base nickel plating, copper plating, semi-bright nickel plating, and bright nickel plating, respectively, and a tertiary counter-current rinsing is performed after each activation treatment.
In one embodiment of the present invention, the process of plating the bottom nickel layer specifically comprises: sulfate nickel plating is carried out, the plating time is 1h, and the current is 30A; the process for plating the semi-bright nickel layer comprises the following specific steps: sulfate nickel plating is carried out, and sulfur-containing additive is added, the plating time is 1h, and the current is 27A; the process for plating the bright nickel layer comprises the following specific steps: sulfate nickel plating, plating time 1h, and current 25A. The copper plating process specifically comprises the following steps: and (3) plating copper by using citrate, wherein the plating time is 1h and the current is 22A.
Compared with the prior art, according to the method for solving the dyne value of the neodymium iron boron product, after the electroplating product is passivated, the cationic surfactant ensures that the passivation solution and the nickel layer are fully hydrophilic, the passivation layer with the thickness of 0.002-0.003mm can be formed within 10 minutes, two components of sodium molybdate and sodium silicate are added into the passivation film, a 32 dyne pen is used for detecting, the dyne value is ensured to be more than 31(N/m), the customer requirement can be met, and the pH stability of the passivation solution is ensured by sodium phosphate, sodium hydroxide and sodium carbonate.
Drawings
Fig. 1 is a flowchart of a method for solving dyne values of an ndfeb product according to an embodiment of the present invention.
Fig. 2A is a dyne value test chart of a neodymium iron boron product which is not treated by the method of the present invention.
Fig. 2B is a dyne value test chart of the ndfeb product processed by the method for solving the dyne value of the ndfeb product of the present invention.
Detailed Description
The following detailed description of the present invention is provided in conjunction with the accompanying drawings, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Throughout the specification and claims, unless explicitly stated otherwise, the word "comprise", or variations such as "comprises" or "comprising", will be understood to imply the inclusion of a stated element or component but not the exclusion of any other element or component.
It should be noted that, the simple testing method of the dyne value is as follows: the product surface is tested directly by the dyne pen, which has the specifications of 32, 36, 38, 40, 42, etc., and represents the corresponding surface tension coefficient, and the numbers 30 and 38 generally represent the surface tension coefficient of the material. The dyne pen 32 format was used in the experiments of the present invention.
As shown in fig. 1, the method for solving the dyne value of the ndfeb product according to the preferred embodiment of the present invention includes the following steps: in step 101, performing electronickelling treatment on the neodymium iron boron product to obtain an electronickelling neodymium iron boron product, wherein the electronickelling treatment comprises plating a bottom nickel layer, plating a copper layer on the bottom nickel layer, plating a semi-bright nickel layer on the copper layer and plating a bright nickel layer on the semi-bright nickel layer to form a total plating layer with the thickness of 0.020-0.025 mm. In step 102, a first secondary counter-current water washing is performed on the nickel-electroplated neodymium iron boron product. In step 103, the neodymium iron boron product subjected to the first secondary counter-current water washing is placed in a passivation solution for passivation treatment, so that a passivation layer with a certain thickness is formed on the surface of the nickel-electroplated neodymium iron boron product, wherein the main components of the passivation solution comprise: cationic surfactant, sodium molybdate, sodium silicate, sodium phosphate, sodium hydroxide and sodium carbonate. In step 104, a second secondary counter-current water wash is performed and a drying process is performed.
In an embodiment of the present invention, wherein, by weight percentage, water: cationic surfactant 1: 0.05; water: sodium molybdate 1: 0.4; water: sodium silicate 1: 0.35; water: sodium phosphate 1: 0.1; water: sodium hydroxide 1: 0.05; water: sodium carbonate 1: 0.1.
In one embodiment of the invention, the passivating solution has a pH of from 10 to 12.
In one embodiment of the present invention, the thickness of the passivation layer is 0.002-0.003 mm.
In one embodiment of the invention, the passivation is performed in a drum with a passivation time of 10min and a drum speed of 11 revolutions per minute.
In one embodiment of the invention, the two-stage countercurrent water washing is carried out by washing in a roller, wherein the washing time of each stage is 17s, and the rotating speed is 11 r/min.
In one embodiment of the present invention, the total thickness of the plated layer of the nickel-plated ndfeb product in step 101 is 0.020-0.025 mm.
In an embodiment of the present invention, the nickel electroplating process in step 101 adopts a nickel-copper-nickel plating process, which specifically includes: carrying out first activation treatment and first cleaning; plating a bottom nickel layer on the neodymium iron boron product subjected to the first activation treatment; carrying out primary secondary recovery to fully recover Ni ions; carrying out second activation treatment and second cleaning; plating a copper layer on the bottom nickel layer; carrying out secondary recovery for the second time to fully recover Cu ions; carrying out third activation treatment and carrying out third cleaning; plating a semi-bright nickel layer on the copper layer; carrying out secondary recovery for the third time to fully recover Ni ions; performing fourth activation treatment and fourth cleaning; plating a bright nickel layer on the semi-bright nickel layer; and step four, performing secondary recovery for the fourth time to fully recover Ni ions and finish the automatic nickel plating process.
In an embodiment of the present invention, the nickel electroplating process in step 101 adopts a nickel-copper-nickel plating process, which specifically includes: first, a first activation treatment is performed, and first cleaning is performed. And then plating a bottom nickel layer on the neodymium iron boron product subjected to the first activation treatment. Then, the first secondary recovery is carried out to sufficiently recover Ni ions. And carrying out second activation treatment and second cleaning. And plating a copper layer on the bottom nickel layer. And carrying out secondary recovery for the second time so as to fully recover the Cu ions. Carrying out third activation treatment and carrying out third cleaning; and plating a semi-bright nickel layer on the copper layer. Carrying out secondary recovery for the third time to fully recover Ni ions; and carrying out fourth activation treatment and carrying out fourth cleaning. Plating a bright nickel layer on the semi-bright nickel layer. And performing secondary recovery for the fourth time to fully recover Ni ions and finish the automatic nickel plating process.
In one embodiment of the present invention, the thickness of the bottom nickel layer, the thickness of the semi-bright nickel layer and the thickness of the bright nickel layer are all in the range of 0.004-0.006 mm. The thickness of the copper plating layer is 0.003-0.005 mm.
In one embodiment of the present invention, the process of plating the bottom nickel layer specifically comprises: sulfate nickel plating is carried out, the plating time is 1h, and the current is 30A; the process for plating the semi-bright nickel layer comprises the following specific steps: sulfate nickel plating is carried out, and sulfur-containing additive is added, the plating time is 1h, and the current is 27A. The process for plating the bright nickel layer comprises the following specific steps: sulfate nickel plating, plating time 1h, and current 25A. The copper plating process specifically comprises the following steps: and (3) plating copper by using citrate, wherein the plating time is 1h and the current is 22A.
In one embodiment of the present invention, three-stage counter-current rinsing is performed before operations of the bottom nickel plating layer, the copper plating layer, the semi-bright nickel plating layer and the bright nickel plating layer, wherein the three-stage counter-current rinsing specifically comprises: after the parts are taken out of the electroplating bath, the parts are firstly cleaned in a first-stage water tank, then cleaned in a second-stage water tank and finally cleaned in a third-stage water tank. At this time, new water is required to overflow from the third-stage water tank to the second-stage water tank, and finally to the first-stage water tank, and is discharged through the overflow groove. Thus, the workpiece motion direction is opposite to the water flow direction. Wherein, each grade of washing time is 17s, and water is automatically added for 17s during roller washing, so that water is saved.
In one embodiment of the invention, the first activation treatment is performed by adding 2% HCl and a corrosion inhibitor, and the activation time is 15 s; the second activation treatment adopts 3 percent HCl and a corrosion inhibitor, and the activation time is 15 s; the third activation treatment adopts 3 percent HCl and a corrosion inhibitor, and the activation time is 15 s; the fourth activation treatment adopts 3 percent HCl and a corrosion inhibitor, and the activation time is 15 s.
In one embodiment of the present invention, the treatment time for the first to fourth secondary recoveries is 17 s.
As shown in FIG. 2B, the dyne value of the Nd-Fe-B product treated by the method of the present invention is 31-40 (N/m), while as shown in FIG. 2A, the dyne value of the product not treated by the method of the present invention is only 25-30 (N/m), therefore, the method of the present invention has the advantages of simple operation, low cost and easy reaching of the dyne value of the product, thereby improving the economic benefit.
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 (8)
1. A method for solving the dyne value of a neodymium-iron-boron product is characterized by comprising the following steps of:
performing electronickelling treatment on the neodymium iron boron product to obtain an electronickelling neodymium iron boron product, wherein the electronickelling treatment comprises a bottom nickel plating layer, a copper plating layer on the bottom nickel plating layer, a semi-bright nickel plating layer on the copper plating layer and a bright nickel plating layer on the semi-bright nickel plating layer;
carrying out primary secondary counter-current water washing on the nickel-electroplated neodymium iron boron product;
placing the neodymium iron boron product subjected to primary secondary countercurrent washing in a passivation solution for passivation treatment, so as to form a passivation layer with a certain thickness on the surface of the nickel-electroplated neodymium iron boron product, wherein the main components of the passivation solution comprise: cationic surfactant, sodium molybdate, sodium silicate, sodium phosphate, sodium hydroxide and sodium carbonate; and
and carrying out secondary countercurrent washing and drying treatment.
2. The method for resolving dyne values of a neodymium iron boron product of claim 1, wherein, in weight percent, water: cationic surfactant 1: 0.05; water: sodium molybdate 1: 0.4; water: sodium silicate 1: 0.35; water: sodium phosphate 1: 0.1; water: sodium hydroxide 1: 0.05; water: sodium carbonate 1: 0.1.
3. The method for solving the dyne value of the neodymium-iron-boron product as claimed in claim 2, wherein the pH value of the passivating solution is 10-12.
4. The method for resolving dyne values of a neodymium iron boron product of claim 1, wherein the thickness of the passivation layer is 0.002-0.003 mm.
5. The method for solving the dyne value of the neodymium-iron-boron product according to claim 1, wherein the passivation treatment is carried out in a roller, the passivation treatment time is 10min, and the rotating speed of the roller is 11 r/min.
6. The method for solving the dyne value of the neodymium iron boron product according to claim 1, wherein the thickness of the bottom nickel layer, the thickness of the semi-bright nickel layer and the thickness of the bright nickel layer are all in the range of 0.004-0.006 mm, and the thickness of the copper plating layer is in the range of 0.003-0.005 mm.
7. The method for solving the dyne value of the neodymium iron boron product according to claim 1, wherein activation treatment and secondary recovery are required to be respectively carried out before and after the base nickel plating, the copper plating, the semi-bright nickel plating and the bright nickel plating, and three-stage countercurrent rinsing is carried out after each activation treatment.
8. The method for solving the dyne value of the neodymium iron boron product according to claim 7, wherein the process for plating the bottom nickel layer specifically comprises the following steps: sulfate nickel plating is carried out, the plating time is 1h, and the current is 30A; the process for plating the semi-bright nickel layer comprises the following specific steps: sulfate nickel plating is carried out, and sulfur-containing additive is added, the plating time is 1h, and the current is 27A; the process for plating the bright nickel layer comprises the following specific steps: sulfate nickel plating, plating time 1h, and current 25A. The copper plating process specifically comprises the following steps: and (3) plating copper by using citrate, wherein the plating time is 1h and the current is 22A.
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| CN111826688A (en) * | 2020-07-10 | 2020-10-27 | 厦门金越电器有限公司 | Electroplating method of samarium-cobalt magnetic steel |
| CN112359382A (en) * | 2020-11-11 | 2021-02-12 | 中钢天源股份有限公司 | Method for reducing heat demagnetization of neodymium iron boron electroplated with nickel, copper and nickel |
| CN112853421A (en) * | 2020-12-31 | 2021-05-28 | 福建省长汀金龙稀土有限公司 | Treating agent capable of improving surface tension of nickel on surface layer of neodymium iron boron and treating method |
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| CN112359382A (en) * | 2020-11-11 | 2021-02-12 | 中钢天源股份有限公司 | Method for reducing heat demagnetization of neodymium iron boron electroplated with nickel, copper and nickel |
| CN112359382B (en) * | 2020-11-11 | 2022-02-18 | 中钢天源股份有限公司 | Method for reducing heat demagnetization of neodymium iron boron electroplated with nickel, copper and nickel |
| CN112853421A (en) * | 2020-12-31 | 2021-05-28 | 福建省长汀金龙稀土有限公司 | Treating agent capable of improving surface tension of nickel on surface layer of neodymium iron boron and treating method |
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Application publication date: 20200626 |