CN110983334A - Neodymium-iron-boron magnet composite nickel plating method - Google Patents
Neodymium-iron-boron magnet composite nickel plating method Download PDFInfo
- Publication number
- CN110983334A CN110983334A CN201911307458.0A CN201911307458A CN110983334A CN 110983334 A CN110983334 A CN 110983334A CN 201911307458 A CN201911307458 A CN 201911307458A CN 110983334 A CN110983334 A CN 110983334A
- Authority
- CN
- China
- Prior art keywords
- iron boron
- neodymium iron
- boron magnet
- chamber
- magnetron sputtering
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/02—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material
- C23C28/023—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings only including layers of metallic material only coatings of metal elements only
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/16—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon
- C23C14/165—Metallic material, boron or silicon on metallic substrates or on substrates of boron or silicon by cathodic sputtering
-
- 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
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Electrochemistry (AREA)
- Manufacturing Cores, Coils, And Magnets (AREA)
- Hard Magnetic Materials (AREA)
Abstract
The invention discloses a neodymium iron boron magnet composite nickel plating method, which comprises the steps of pretreating a neodymium iron boron magnet, then carrying out continuous magnetron sputtering nickel plating treatment on the pretreated neodymium iron boron magnet, and finally carrying out electroplating chemical nickel treatment on the neodymium iron boron magnet after the continuous magnetron sputtering nickel plating treatment; the method has the advantages that a compact sputtering nickel layer is formed on the surface of the neodymium iron boron magnet body through continuous magnetron sputtering nickel plating treatment, a compact electroplating nickel layer is formed on the surface of the sputtering nickel layer through electroplating chemical nickel treatment, the neodymium iron boron magnet body is guaranteed to have high corrosion resistance and wear resistance, no sharp point effect exists in the magnetron sputtering treatment process and the electroplating chemical nickel treatment process, the uniformity of a composite coating formed by the sputtering nickel layer and the electroplating nickel layer is good, the size of a product is easy to control, continuous magnetron sputtering nickel plating is adopted, the electroplating process is shortened, and waste water is reduced by 70%.
Description
Technical Field
The invention relates to a nickel plating method, in particular to a neodymium iron boron magnet composite nickel plating method.
Background
The neodymium iron boron magnet has excellent magnetic performance and high cost performance, and is widely applied to the technical fields of electronics, motors, communication and the like. However, the neodymium iron boron magnet is very active and is easily corroded, so that the problems of rusting, pulverization or loss of magnetism are caused, and the service life and the application field of the neodymium iron boron magnet are greatly limited.
At present, the surface of the neodymium iron boron magnet is mainly subjected to electroplating treatment to improve the corrosion resistance, wherein an electroplated nickel layer is widely used due to excellent temperature resistance and wear resistance. The existing nickel plating method for the neodymium iron boron magnet is usually to hang the neodymium iron boron magnet on a hanger and then put the neodymium iron boron magnet into an electric aqueduct for electroplating. However, the conventional nickel plating method for the neodymium iron boron magnet has the following problems: firstly, the dog bone effect of the rack plating product is obvious, if the minimum plating thickness of the product is ensured to be 25 mu m, the plating thickness of the corner plating of part of the product is up to 100 mu m, the size of the product is not easy to control, and the plating uniformity is poor; secondly, the rack-plated nickel layer has large crystal particles, poor compactness and poor corrosion resistance, and the corrosion resistance of the nickel layer needs to be improved by increasing the thickness of the plating layer, so that the thickness of the nickel layer is larger; thirdly, the flow of the electroplating process is long, the washing process is more, and the amount of waste water is large.
Disclosure of Invention
The invention aims to solve the technical problem of providing a neodymium iron boron magnet composite nickel plating method which is easy to control the size of a product, good in coating thickness uniformity, smaller in coating thickness on the basis of higher corrosion resistance, shorter in process flow and less in waste water.
The technical scheme adopted by the invention for solving the technical problems is as follows: a composite nickel plating method for a neodymium iron boron magnet comprises the following steps:
① preprocessing the Nd-Fe-B magnet;
② continuous magnetron sputtering nickel plating treatment is carried out on the pretreated neodymium iron boron magnet;
③ the neodymium iron boron magnet after the continuous magnetron sputtering nickel plating treatment is processed by the electroplating chemical nickel treatment.
The specific process of carrying out continuous magnetron sputtering nickel plating treatment on the pretreated neodymium iron boron magnet is as follows:
② -1, building a processing chamber required in the process of carrying out continuous magnetron sputtering nickel plating on the pretreated neodymium iron boron magnet, wherein the processing chamber comprises five working chambers which are sequentially arranged from front to back, a closed door is arranged between every two adjacent working chambers, when the closed door arranged between the two adjacent working chambers is opened, the two adjacent working chambers are communicated, and when the closed door arranged between the two adjacent working chambers is closed, the two adjacent working chambers are isolated;
an automatic transmission device is arranged to penetrate through five working chambers, the five working chambers are sequentially called a feeding chamber, a preheating chamber, a magnetron sputtering chamber, a cooling chamber and a discharging chamber from front to back,
② -2 placing NdFeB magnets on the screen plate at intervals, wherein the distance between every two adjacent NdFeB magnets is larger than the thickness of the NdFeB magnets;
② -3 feeding the neodymium-iron-boron magnet-containing net plate into the feeding chamber by automatic conveying equipment, sealing the feeding chamber, and vacuumizing to less than or equal to 2.0 × 10-3Pa；
② -4, opening a sealing door between the feeding chamber and the preheating chamber, sending the neodymium iron boron magnet in the feeding chamber into the preheating chamber by automatic conveying equipment, sealing the sealing door between the feeding chamber and the preheating chamber again, and pre-drying the neodymium iron boron magnet in the preheating chamber by adopting pre-drying equipment, wherein the pre-drying temperature is 100-;
② -5, opening a closed door between the preheating chamber and the magnetron sputtering chamber, sending the preheated neodymium iron boron magnet into the magnetron sputtering chamber by automatic conveying equipment, then closing the closed door between the magnetron sputtering chamber and the preheating chamber again, and carrying out magnetron sputtering treatment on the neodymium iron boron magnet in the magnetron sputtering chamber by magnetron sputtering equipment, wherein the magnetron sputtering treatment target material adopts nickel, the target power is 200-400W, the air pressure is 0.1-0.3Pa, the thickness of a sputtering film layer formed on the surface of the neodymium iron boron magnet is 3-8 μm, and the treatment time is 10-20 minutes;
② -6, opening a closed door between the magnetron sputtering chamber and the cooling chamber, conveying the neodymium iron boron magnet subjected to magnetron sputtering into the cooling chamber by automatic conveying equipment, closing the closed door between the magnetron sputtering chamber and the cooling chamber, and cooling the neodymium iron boron magnet to below 80 ℃ in the cooling chamber by adopting cooling equipment;
② -7, opening a sealing door between the cooling chamber and the discharging chamber, sending the cooled neodymium-iron-boron magnet into the discharging chamber by automatic conveying equipment, sealing the sealing door between the cooling chamber and the discharging chamber, and taking out the screen plate from the discharging chamber;
② -8 placing the neodymium iron boron magnets on the screen plate at intervals after turning over, wherein the interval distance between every two adjacent neodymium iron boron magnets is larger than the thickness of the neodymium iron boron magnets;
② -9, reprocessing the NdFeB magnet according to the method of the step ② -3- ② -7 to obtain the NdFeB magnet after the continuous magnetron sputtering nickel plating treatment, wherein the continuous magnetron sputtering nickel plating treatment adopts a continuous production flow, the production tact can be 40 min/screen plate, compared with the conventional magnetron sputtering nickel plating process, the process flow is shorter, the production efficiency is greatly improved, and the requirement of rapid production can be met.
The specific process for carrying out the electroplating chemical nickel treatment on the neodymium iron boron magnet subjected to the continuous magnetron sputtering nickel plating treatment comprises the following steps:
③ -1, loading the neodymium iron boron magnet after continuous magnetron sputtering nickel plating treatment into a roller, and performing activation treatment by using a sulfuric acid solution, wherein the sulfuric acid solution is formed by uniformly mixing sulfuric acid and water, the mass percentage of the sulfuric acid in the sulfuric acid solution is 2-3%, and the rotating speed of the roller is 2-4r/min in the activation treatment process;
③ -2, washing the activated neodymium iron boron magnet twice in sequence, wherein both washing are carried out in a roller, and the rotating speed of the roller is 2-4 r/min;
③ -3, electroplating the neodymium iron boron magnet which is washed by water twice by adopting an electroplating solution with the pH value of 4.5-5.0, wherein the temperature of the electroplating solution is 88-93 ℃, the electroplating solution is formed by uniformly mixing nickel sulfate, sodium hypophosphite, sodium acetate, sodium citrate and water, the concentration of nickel sulfate is 25-32g/L, the concentration of sodium hypophosphite is 20-30g/L, the concentration of sodium acetate is 10-20g/L, and the concentration of sodium citrate is 8-12g/L, and after the electroplating is finished, a chemical nickel layer with the thickness of 4-8 mu m is formed on the surface of a sputtering film layer;
③ -4, washing for three times in the roller in sequence, wherein the rotating speed of the roller is 2-4 r/min;
③ -5, washing the neodymium iron boron magnet by adopting an oxalic acid solution, wherein the oxalic acid solution is formed by uniformly mixing oxalic acid and water, and the concentration of the oxalic acid in the oxalic acid solution is 1-3 g/L;
③ -6, the chemical nickel treatment is completed after two times of water washing, the chemical nickel electroplating treatment process is used as an auxiliary process of the continuous magnetron sputtering nickel plating treatment process, and a plating layer is formed on the surface of the sputtering film layer again, so that the corrosion resistance and the wear resistance of the product are enhanced, and the uniformity of the plating layer is ensured.
The specific process of the pretreatment comprises the following steps:
① -1, carrying out alkaline degreasing treatment on the neodymium iron boron magnet at the temperature of 50-70 ℃;
① -2, washing the alkaline degreased neodymium iron boron magnet twice;
① -3, pickling the neodymium iron boron magnet by nitric acid pickling solution at room temperature, wherein the nitric acid pickling solution is formed by uniformly mixing nitric acid and water, and the mass percentage of the nitric acid in the nitric acid pickling solution is 5-7%;
① -4, washing the acid-washed neodymium iron boron magnet twice;
① -5, placing the neodymium iron boron magnet into ultrasonic deoiling liquid, and performing ultrasonic deoiling treatment by using ultrasonic equipment, wherein the ultrasonic deoiling liquid is formed by uniformly mixing potassium pyrophosphate, sodium carbonate, OP emulsifier and water, the concentration of potassium pyrophosphate is 40-60g/L, the concentration of sodium carbonate is 5-15g/L, and the concentration of OP emulsifier is 0.4-1.0 ml/L;
① -6 washing the Nd-Fe-B magnet twice;
① -7, carrying out ultrasonic water washing on the neodymium iron boron magnet;
① -8, cleaning the neodymium iron boron magnet by alcohol, then drying, and finishing the pretreatment.
Compared with the prior art, the invention has the advantages that the neodymium iron boron magnet is pretreated, then the pretreated neodymium iron boron magnet is subjected to continuous magnetron sputtering nickel plating treatment to form a compact sputtering nickel layer on the surface of the neodymium iron boron magnet, finally the neodymium iron boron magnet subjected to the continuous magnetron sputtering nickel plating treatment is subjected to electroplating chemical nickel treatment, and a compact electroplating nickel layer is formed on the surface of the sputtering nickel layer through chemical nickel deposition, so that the neodymium iron boron magnet has higher corrosion resistance and wear resistance, the magnetron sputtering treatment process and the electroplating chemical nickel treatment process have no sharp point effect, the composite plating layer formed by the sputtering nickel layer and the electroplating nickel layer has good uniformity and easily controlled product size, and the continuous magnetron sputtering nickel plating is adopted to shorten the electroplating process, the waste water is reduced by more than 70 percent, and the neodymium iron boron magnet treated by adopting the method of the invention is compared with the neodymium iron boron magnet treated by the prior art, the corrosion resistance test is carried out for 160h with the duration of 120-.
Detailed Description
The present invention will be described in further detail with reference to examples.
The first embodiment is as follows: a composite nickel plating method for a neodymium iron boron magnet comprises the following steps:
① preprocessing the Nd-Fe-B magnet;
② continuous magnetron sputtering nickel plating treatment is carried out on the pretreated neodymium iron boron magnet;
③ the neodymium iron boron magnet after the continuous magnetron sputtering nickel plating treatment is processed by the electroplating chemical nickel treatment.
In this embodiment, the specific process of performing the continuous magnetron sputtering nickel plating treatment on the pretreated ndfeb magnet is as follows:
② -1, building a processing chamber required in the process of carrying out continuous magnetron sputtering nickel plating on the pretreated neodymium iron boron magnet, wherein the processing chamber comprises five working chambers which are sequentially arranged from front to back, a closed door is arranged between every two adjacent working chambers, when the closed door arranged between the two adjacent working chambers is opened, the two adjacent working chambers are communicated, and when the closed door arranged between the two adjacent working chambers is closed, the two adjacent working chambers are isolated;
an automatic transmission device is arranged to penetrate through five working chambers, the five working chambers are sequentially called a feeding chamber, a preheating chamber, a magnetron sputtering chamber, a cooling chamber and a discharging chamber from front to back,
② -2 placing NdFeB magnets on the screen plate at intervals, wherein the distance between every two adjacent NdFeB magnets is larger than the thickness of the NdFeB magnets;
② -3 feeding the neodymium-iron-boron magnet-containing net plate into the feeding chamber by automatic conveying equipment, sealing the feeding chamber, and vacuumizing to 2.0 × 10-3Pa；
② -4, opening a sealing door between the feeding chamber and the preheating chamber, conveying the neodymium iron boron magnet in the feeding chamber into the preheating chamber by automatic conveying equipment, sealing the sealing door between the feeding chamber and the preheating chamber again, and pre-drying the neodymium iron boron magnet in the preheating chamber by adopting pre-drying equipment, wherein the pre-drying temperature is 100 ℃, and the pre-drying time is 10 minutes;
② -5, opening a closed door between the preheating chamber and the magnetron sputtering chamber, sending the preheated neodymium iron boron magnet into the magnetron sputtering chamber by automatic conveying equipment, then closing the closed door between the magnetron sputtering chamber and the preheating chamber again, and carrying out magnetron sputtering treatment on the neodymium iron boron magnet in the magnetron sputtering chamber by magnetron sputtering equipment, wherein the magnetron sputtering treatment target material adopts nickel, the target power is 200W, the air pressure is 0.1Pa, the thickness of a sputtering film layer formed on the surface of the neodymium iron boron magnet is 3-8 μm, and the treatment time is 10 minutes;
② -6, opening a closed door between the magnetron sputtering chamber and the cooling chamber, conveying the neodymium iron boron magnet subjected to magnetron sputtering into the cooling chamber by automatic conveying equipment, closing the closed door between the magnetron sputtering chamber and the cooling chamber, and cooling the neodymium iron boron magnet to below 80 ℃ in the cooling chamber by adopting cooling equipment;
② -7, opening a sealing door between the cooling chamber and the discharging chamber, sending the cooled neodymium-iron-boron magnet into the discharging chamber by automatic conveying equipment, sealing the sealing door between the cooling chamber and the discharging chamber, and taking out the screen plate from the discharging chamber;
② -8 placing the neodymium iron boron magnets on the screen plate at intervals after turning over, wherein the interval distance between every two adjacent neodymium iron boron magnets is larger than the thickness of the neodymium iron boron magnets;
② -9, the neodymium iron boron magnet is processed again according to the method of steps ② -3- ② -7, and the neodymium iron boron magnet after the continuous magnetron sputtering nickel plating treatment is obtained.
In this embodiment, the specific process of performing the chemical nickel electroplating treatment on the neodymium iron boron magnet after the continuous magnetron sputtering nickel plating treatment is as follows:
③ -1, loading the neodymium iron boron magnet after the continuous magnetron sputtering nickel plating treatment into a roller, and performing activation treatment by adopting a sulfuric acid solution, wherein the sulfuric acid solution is formed by uniformly mixing sulfuric acid and water, the mass percentage of the sulfuric acid in the sulfuric acid solution is 2%, and the rotating speed of the roller is 2r/min in the activation treatment process;
③ -2, washing the activated neodymium iron boron magnet twice in sequence, wherein both washing are carried out in a roller, and the rotating speed of the roller is 2 r/min;
③ -3, electroplating the neodymium iron boron magnet which is washed twice with water by adopting an electroplating solution with the pH value of 4.5, wherein the temperature of the electroplating solution is 88 ℃, the electroplating solution is formed by uniformly mixing nickel sulfate, sodium hypophosphite, sodium acetate, sodium citrate and water, the concentration of nickel sulfate in the electroplating solution is 25g/L, the concentration of sodium hypophosphite is 20g/L, the concentration of sodium acetate is 10g/L, and the concentration of sodium citrate is 8g/L, and after the electroplating is finished, a chemical nickel layer with the thickness of 4 mu m is formed on the surface of a sputtering film layer;
③ -4, washing for three times in the roller in sequence, wherein the rotating speed of the roller is 2 r/min;
③ -5, washing the neodymium iron boron magnet by adopting an oxalic acid solution, wherein the oxalic acid solution is formed by uniformly mixing oxalic acid and water, and the concentration of the oxalic acid in the oxalic acid solution is 1 g/L;
③ -6, two times of water washing are carried out in sequence, and the chemical nickel treatment is completed.
In this embodiment, the specific process of the pretreatment is as follows:
① -1, carrying out alkaline degreasing treatment on the neodymium iron boron magnet at the temperature of 50 ℃;
① -2, washing the alkaline degreased neodymium iron boron magnet twice;
① -3, pickling the neodymium iron boron magnet by nitric acid pickling solution at room temperature, wherein the nitric acid pickling solution is formed by uniformly mixing nitric acid and water, and the mass percentage of the nitric acid in the nitric acid pickling solution is 5%;
① -4, washing the acid-washed neodymium iron boron magnet twice;
① -5, placing the neodymium iron boron magnet into ultrasonic deoiling liquid, and performing ultrasonic deoiling treatment by using ultrasonic equipment, wherein the ultrasonic deoiling liquid is formed by uniformly mixing potassium pyrophosphate, sodium carbonate, OP emulsifier and water, and the concentration of potassium pyrophosphate, sodium carbonate and OP emulsifier in the ultrasonic deoiling liquid is 40g/L, 5g/L and 0.4ml/L respectively;
① -6 washing the Nd-Fe-B magnet twice;
① -7, carrying out ultrasonic water washing on the neodymium iron boron magnet;
① -8, cleaning the neodymium iron boron magnet by alcohol, then drying the magnet by blowing, and finishing the pretreatment.
Example two: a composite nickel plating method for a neodymium iron boron magnet comprises the following steps:
① preprocessing the Nd-Fe-B magnet;
② continuous magnetron sputtering nickel plating treatment is carried out on the pretreated neodymium iron boron magnet;
③ the neodymium iron boron magnet after the continuous magnetron sputtering nickel plating treatment is processed by the electroplating chemical nickel treatment.
In this embodiment, the specific process of performing the continuous magnetron sputtering nickel plating treatment on the pretreated ndfeb magnet is as follows:
② -1, building a processing chamber required in the process of carrying out continuous magnetron sputtering nickel plating on the pretreated neodymium iron boron magnet, wherein the processing chamber comprises five working chambers which are sequentially arranged from front to back, a closed door is arranged between every two adjacent working chambers, when the closed door arranged between the two adjacent working chambers is opened, the two adjacent working chambers are communicated, and when the closed door arranged between the two adjacent working chambers is closed, the two adjacent working chambers are isolated;
an automatic transmission device is arranged to penetrate through five working chambers, the five working chambers are sequentially called a feeding chamber, a preheating chamber, a magnetron sputtering chamber, a cooling chamber and a discharging chamber from front to back,
② -2 placing NdFeB magnets on the screen plate at intervals, wherein the distance between every two adjacent NdFeB magnets is larger than the thickness of the NdFeB magnets;
② -3 feeding the neodymium-iron-boron magnet-containing net plate into the feeding chamber by automatic conveying equipment, sealing the feeding chamber, and vacuumizing to 2.0 × 10-3Pa；
② -4, opening a sealing door between the feeding chamber and the preheating chamber, conveying the neodymium iron boron magnet in the feeding chamber into the preheating chamber by automatic conveying equipment, sealing the sealing door between the feeding chamber and the preheating chamber again, and pre-drying the neodymium iron boron magnet in the preheating chamber by adopting pre-drying equipment, wherein the pre-drying temperature is 120 ℃ and the pre-drying time is 20 minutes;
② -5, opening a closed door between the preheating chamber and the magnetron sputtering chamber, sending the preheated neodymium iron boron magnet into the magnetron sputtering chamber by automatic conveying equipment, then closing the closed door between the magnetron sputtering chamber and the preheating chamber again, and carrying out magnetron sputtering treatment on the neodymium iron boron magnet in the magnetron sputtering chamber by magnetron sputtering equipment, wherein the magnetron sputtering treatment target material adopts nickel, the target power is 400W, the air pressure is 0.3Pa, the thickness of a sputtering film layer formed on the surface of the neodymium iron boron magnet is 3-8 μm, and the treatment time is 20 minutes;
② -6, opening a closed door between the magnetron sputtering chamber and the cooling chamber, conveying the neodymium iron boron magnet subjected to magnetron sputtering into the cooling chamber by automatic conveying equipment, closing the closed door between the magnetron sputtering chamber and the cooling chamber, and cooling the neodymium iron boron magnet to below 80 ℃ in the cooling chamber by adopting cooling equipment;
② -7, opening a sealing door between the cooling chamber and the discharging chamber, sending the cooled neodymium-iron-boron magnet into the discharging chamber by automatic conveying equipment, sealing the sealing door between the cooling chamber and the discharging chamber, and taking out the screen plate from the discharging chamber;
② -8 placing the neodymium iron boron magnets on the screen plate at intervals after turning over, wherein the interval distance between every two adjacent neodymium iron boron magnets is larger than the thickness of the neodymium iron boron magnets;
② -9, the neodymium iron boron magnet is processed again according to the method of steps ② -3- ② -7, and the neodymium iron boron magnet after the continuous magnetron sputtering nickel plating treatment is obtained.
In this embodiment, the specific process of performing the chemical nickel electroplating treatment on the neodymium iron boron magnet after the continuous magnetron sputtering nickel plating treatment is as follows:
③ -1, loading the neodymium iron boron magnet after the continuous magnetron sputtering nickel plating treatment into a roller, and performing activation treatment by using a sulfuric acid solution, wherein the sulfuric acid solution is formed by uniformly mixing sulfuric acid and water, the mass percentage of the sulfuric acid in the sulfuric acid solution is 3%, and the rotating speed of the roller is 4r/min in the activation treatment process;
③ -2, washing the activated neodymium iron boron magnet twice in sequence, wherein both washing are carried out in a roller, and the rotating speed of the roller is 4 r/min;
③ -3, electroplating the neodymium iron boron magnet which is washed twice with water by adopting an electroplating solution with the pH value of 5.0, wherein the temperature of the electroplating solution is 93 ℃, the electroplating solution is formed by uniformly mixing nickel sulfate, sodium hypophosphite, sodium acetate, sodium citrate and water, the concentration of nickel sulfate in the electroplating solution is 32g/L, the concentration of sodium hypophosphite is 30g/L, the concentration of sodium acetate is 20g/L, and the concentration of sodium citrate is 12g/L, and after the electroplating is finished, a chemical nickel layer with the thickness of 8 mu m is formed on the surface of a sputtering film layer;
③ -4, washing for three times in the roller in sequence, wherein the rotating speed of the roller is 4 r/min;
③ -5, washing the neodymium iron boron magnet by adopting an oxalic acid solution, wherein the oxalic acid solution is formed by uniformly mixing oxalic acid and water, and the concentration of the oxalic acid in the oxalic acid solution is 3 g/L;
③ -6, two times of water washing are carried out in sequence, and the chemical nickel treatment is completed.
In this embodiment, the specific process of the pretreatment is as follows:
① -1, carrying out alkaline degreasing treatment on the neodymium iron boron magnet at the temperature of 70 ℃;
① -2, washing the alkaline degreased neodymium iron boron magnet twice;
① -3, pickling the neodymium iron boron magnet by nitric acid pickling solution at room temperature, wherein the nitric acid pickling solution is formed by uniformly mixing nitric acid and water, and the mass percentage of the nitric acid in the nitric acid pickling solution is 7%;
① -4, washing the acid-washed neodymium iron boron magnet twice;
① -5, placing the neodymium iron boron magnet into ultrasonic deoiling liquid, and performing ultrasonic deoiling treatment by using ultrasonic equipment, wherein the ultrasonic deoiling liquid is formed by uniformly mixing potassium pyrophosphate, sodium carbonate, OP emulsifier and water, the concentration of potassium pyrophosphate is 60g/L, the concentration of sodium carbonate is 15g/L, and the concentration of OP emulsifier is 1.0 ml/L;
① -6 washing the Nd-Fe-B magnet twice;
① -7, carrying out ultrasonic water washing on the neodymium iron boron magnet;
① -8, cleaning the neodymium iron boron magnet by alcohol, then drying the magnet by blowing, and finishing the pretreatment.
The corrosion resistance of the neodymium iron boron magnet treated by the method is tested, the corrosion resistance test is endured for 160h with 120-fold, and compared with the conventional nickel plating method for the neodymium iron boron magnet, the corrosion resistance test is improved by 2.5-10 times, the service life is long, the operation reliability is high, and the application field is wide.
Claims (4)
1. A composite nickel plating method for a neodymium iron boron magnet is characterized by comprising the following steps:
① preprocessing the Nd-Fe-B magnet;
② continuous magnetron sputtering nickel plating treatment is carried out on the pretreated neodymium iron boron magnet;
③ the neodymium iron boron magnet after the continuous magnetron sputtering nickel plating treatment is processed by the electroplating chemical nickel treatment.
2. The method for composite nickel plating on the neodymium iron boron magnet according to claim 1, characterized in that the specific process for carrying out continuous magnetron sputtering nickel plating treatment on the pretreated neodymium iron boron magnet comprises the following steps:
② -1, building a processing chamber required in the process of carrying out continuous magnetron sputtering nickel plating on the pretreated neodymium iron boron magnet, wherein the processing chamber comprises five working chambers which are sequentially arranged from front to back, a closed door is arranged between every two adjacent working chambers, when the closed door arranged between the two adjacent working chambers is opened, the two adjacent working chambers are communicated, and when the closed door arranged between the two adjacent working chambers is closed, the two adjacent working chambers are isolated;
an automatic transmission device is arranged to penetrate through five working chambers, the five working chambers are sequentially called a feeding chamber, a preheating chamber, a magnetron sputtering chamber, a cooling chamber and a discharging chamber from front to back,
② -2 placing NdFeB magnets on the screen plate at intervals, wherein the distance between every two adjacent NdFeB magnets is larger than the thickness of the NdFeB magnets;
② -3 feeding the neodymium-iron-boron magnet-containing net plate into the feeding chamber by automatic conveying equipment, sealing the feeding chamber, and vacuumizing to 2.0 × 10-3Pa；
② -4, opening a sealing door between the feeding chamber and the preheating chamber, sending the neodymium iron boron magnet in the feeding chamber into the preheating chamber by automatic conveying equipment, sealing the sealing door between the feeding chamber and the preheating chamber again, and pre-drying the neodymium iron boron magnet in the preheating chamber by adopting pre-drying equipment, wherein the pre-drying temperature is 100-;
② -5, opening a closed door between the preheating chamber and the magnetron sputtering chamber, sending the preheated neodymium iron boron magnet into the magnetron sputtering chamber by automatic conveying equipment, then closing the closed door between the magnetron sputtering chamber and the preheating chamber again, and carrying out magnetron sputtering treatment on the neodymium iron boron magnet in the magnetron sputtering chamber by magnetron sputtering equipment, wherein the magnetron sputtering treatment target material adopts nickel, the target power is 200-400W, the air pressure is 0.1-0.3Pa, the thickness of a sputtering film layer formed on the surface of the neodymium iron boron magnet is 3-8 μm, and the treatment time is 10-20 minutes;
② -6, opening a closed door between the magnetron sputtering chamber and the cooling chamber, conveying the neodymium iron boron magnet subjected to magnetron sputtering into the cooling chamber by automatic conveying equipment, closing the closed door between the magnetron sputtering chamber and the cooling chamber, and cooling the neodymium iron boron magnet to below 80 ℃ in the cooling chamber by adopting cooling equipment;
② -7, opening a sealing door between the cooling chamber and the discharging chamber, sending the cooled neodymium-iron-boron magnet into the discharging chamber by automatic conveying equipment, sealing the sealing door between the cooling chamber and the discharging chamber, and taking out the screen plate from the discharging chamber;
② -8 placing the neodymium iron boron magnets on the screen plate at intervals after turning over, wherein the interval distance between every two adjacent neodymium iron boron magnets is larger than the thickness of the neodymium iron boron magnets;
② -9, the neodymium iron boron magnet is processed again according to the method of steps ② -3- ② -7, and the neodymium iron boron magnet after the continuous magnetron sputtering nickel plating treatment is obtained.
3. The composite nickel plating method for the neodymium iron boron magnet according to claim 1, characterized in that the specific process of performing the chemical nickel electroplating treatment on the neodymium iron boron magnet after the continuous magnetron sputtering nickel plating treatment comprises the following steps:
③ -1, loading the neodymium iron boron magnet after continuous magnetron sputtering nickel plating treatment into a roller, and performing activation treatment by using a sulfuric acid solution, wherein the sulfuric acid solution is formed by uniformly mixing sulfuric acid and water, the mass percentage of the sulfuric acid in the sulfuric acid solution is 2-3%, and the rotating speed of the roller is 2-4r/min in the activation treatment process;
③ -2, washing the activated neodymium iron boron magnet twice in sequence, wherein both washing are carried out in a roller, and the rotating speed of the roller is 2-4 r/min;
③ -3, electroplating the neodymium iron boron magnet which is washed by water twice by adopting an electroplating solution with the pH value of 4.5-5.0, wherein the temperature of the electroplating solution is 88-93 ℃, the electroplating solution is formed by uniformly mixing nickel sulfate, sodium hypophosphite, sodium acetate, sodium citrate and water, the concentration of nickel sulfate is 25-32g/L, the concentration of sodium hypophosphite is 20-30g/L, the concentration of sodium acetate is 10-20g/L, and the concentration of sodium citrate is 8-12g/L, and after the electroplating is finished, a chemical nickel layer with the thickness of 4-8 mu m is formed on the surface of a sputtering film layer;
③ -4, washing for three times in the roller in sequence, wherein the rotating speed of the roller is 2-4 r/min;
③ -5, washing the neodymium iron boron magnet by adopting an oxalic acid solution, wherein the oxalic acid solution is formed by uniformly mixing oxalic acid and water, and the concentration of the oxalic acid in the oxalic acid solution is 1-3 g/L;
③ -6, two times of water washing are carried out in sequence, and the chemical nickel treatment is completed.
4. The method for composite nickel plating on neodymium iron boron magnet according to claim 1, characterized in that the specific process of the pretreatment is as follows:
① -1, carrying out alkaline degreasing treatment on the neodymium iron boron magnet at the temperature of 50-70 ℃;
① -2, washing the alkaline degreased neodymium iron boron magnet twice;
① -3, pickling the neodymium iron boron magnet by nitric acid pickling solution at room temperature, wherein the nitric acid pickling solution is formed by uniformly mixing nitric acid and water, and the mass percentage of the nitric acid in the nitric acid pickling solution is 5-7%;
① -4, washing the acid-washed neodymium iron boron magnet twice;
① -5, placing the neodymium iron boron magnet into ultrasonic deoiling liquid, and performing ultrasonic deoiling treatment by using ultrasonic equipment, wherein the ultrasonic deoiling liquid is formed by uniformly mixing potassium pyrophosphate, sodium carbonate, OP emulsifier and water, the concentration of potassium pyrophosphate is 40-60g/L, the concentration of sodium carbonate is 5-15g/L, and the concentration of OP emulsifier is 0.4-1.0 ml/L;
① -6 washing the Nd-Fe-B magnet twice;
① -7, carrying out ultrasonic water washing on the neodymium iron boron magnet;
① -8, cleaning the neodymium iron boron magnet by alcohol, then drying the magnet by blowing, and finishing the pretreatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911307458.0A CN110983334A (en) | 2019-12-18 | 2019-12-18 | Neodymium-iron-boron magnet composite nickel plating method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911307458.0A CN110983334A (en) | 2019-12-18 | 2019-12-18 | Neodymium-iron-boron magnet composite nickel plating method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110983334A true CN110983334A (en) | 2020-04-10 |
Family
ID=70095201
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911307458.0A Pending CN110983334A (en) | 2019-12-18 | 2019-12-18 | Neodymium-iron-boron magnet composite nickel plating method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110983334A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111962132A (en) * | 2020-08-11 | 2020-11-20 | 龚兴娅 | Continuous electroplating device for producing neodymium iron boron magnet and implementation method thereof |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1807686A (en) * | 2006-02-16 | 2006-07-26 | 浙江大学 | Surface anti-rust treatment method for powder moulded permanent magnet |
| CN102628163A (en) * | 2012-04-20 | 2012-08-08 | 成都中光电阿波罗太阳能有限公司 | Cadmium telluride thin-film solar cell back contact layer production method and vertical coater |
| CN202702728U (en) * | 2012-04-12 | 2013-01-30 | 天津市日达成稀土科技有限公司 | Neodymium iron boron (NdFeB) magnet surface electroplating and chemical plating composite plate structure |
| CN103173763A (en) * | 2013-03-28 | 2013-06-26 | 宁波韵升股份有限公司 | Electroplating and vapor deposition composite protection method for neodymium-iron-boron magnet |
| CN105420669A (en) * | 2015-11-29 | 2016-03-23 | 中国人民解放军装甲兵工程学院 | Vapor deposition method used for anticorrosion pretreatment of permanent magnet |
| CN106282948A (en) * | 2016-07-28 | 2017-01-04 | 北京中科三环高技术股份有限公司 | A kind of film plating process and coating system and the preparation method of rare-earth magnet |
| CN208917290U (en) * | 2018-05-02 | 2019-05-31 | 北京七星华创集成电路装备有限公司 | A kind of magnetic-control sputtering continuous plating equipment |
| CN209412302U (en) * | 2018-10-17 | 2019-09-20 | 苏州善柔真空科技有限公司 | A kind of vacuum coating system of the compound PVD of vertical PECVD |
-
2019
- 2019-12-18 CN CN201911307458.0A patent/CN110983334A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1807686A (en) * | 2006-02-16 | 2006-07-26 | 浙江大学 | Surface anti-rust treatment method for powder moulded permanent magnet |
| CN202702728U (en) * | 2012-04-12 | 2013-01-30 | 天津市日达成稀土科技有限公司 | Neodymium iron boron (NdFeB) magnet surface electroplating and chemical plating composite plate structure |
| CN102628163A (en) * | 2012-04-20 | 2012-08-08 | 成都中光电阿波罗太阳能有限公司 | Cadmium telluride thin-film solar cell back contact layer production method and vertical coater |
| CN103173763A (en) * | 2013-03-28 | 2013-06-26 | 宁波韵升股份有限公司 | Electroplating and vapor deposition composite protection method for neodymium-iron-boron magnet |
| CN105420669A (en) * | 2015-11-29 | 2016-03-23 | 中国人民解放军装甲兵工程学院 | Vapor deposition method used for anticorrosion pretreatment of permanent magnet |
| CN106282948A (en) * | 2016-07-28 | 2017-01-04 | 北京中科三环高技术股份有限公司 | A kind of film plating process and coating system and the preparation method of rare-earth magnet |
| CN208917290U (en) * | 2018-05-02 | 2019-05-31 | 北京七星华创集成电路装备有限公司 | A kind of magnetic-control sputtering continuous plating equipment |
| CN209412302U (en) * | 2018-10-17 | 2019-09-20 | 苏州善柔真空科技有限公司 | A kind of vacuum coating system of the compound PVD of vertical PECVD |
Non-Patent Citations (2)
| Title |
|---|
| 朱庚惠等: "《中级电镀工工艺学》", 31 October 1988, 机械工业出版社 * |
| 沈亚光: "《防护与装饰性电镀》", 30 November 2008, 国防工业出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111962132A (en) * | 2020-08-11 | 2020-11-20 | 龚兴娅 | Continuous electroplating device for producing neodymium iron boron magnet and implementation method thereof |
| CN111962132B (en) * | 2020-08-11 | 2021-10-19 | 包头市英思特稀磁新材料股份有限公司 | Continuous electroplating device for producing neodymium iron boron magnet and implementation method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105336490B (en) | A kind of processing method of Nd-Fe-B permanent magnet | |
| CN106968003A (en) | Nd-Fe-B magnet steel overlay coating method | |
| EP3486925B1 (en) | Ndfeb magnet with composite coating and preparation process thereof | |
| CN105970197B (en) | A kind of kirsite chemical bronze plating liquid and application | |
| US9783883B2 (en) | Method for depositing aluminum on a permanent Nd—Fe—B magnet | |
| CN109256256B (en) | Neodymium-iron-boron magnet with zinc-nickel alloy electroplated on surface and preparation process thereof | |
| CN101736304B (en) | Vacuum aluminizing method of surface of neodymium-iron-boron permanent magnet | |
| CN103173763A (en) | Electroplating and vapor deposition composite protection method for neodymium-iron-boron magnet | |
| CN112899684A (en) | Neodymium iron boron magnet copper nickel electroplating process | |
| CN104120470B (en) | Steel and iron parts or zinc alloy diecasting are without the cyanogen pre-leaching copper method of monovalence copper | |
| CN110983334A (en) | Neodymium-iron-boron magnet composite nickel plating method | |
| CN104073849A (en) | Technique for electroplating nickel-tungsten-phosphorus on surface of sintered neodymium-iron-boron magnet | |
| CN101550570A (en) | Non-cyanide electro cooper plating bath of EDTA system and use method thereof | |
| CN103014798A (en) | Electrochromism processing method for iron-based powder metallurgic part | |
| CN105040004B (en) | A kind of Sintered NdFeB magnet surface coating technique | |
| CN103757632A (en) | Surface treatment method for permanent magnet material and permanent magnet material | |
| CN109136864B (en) | Method for vacuum coating of aluminum-tin composite coating on surface of magnetic steel | |
| CN114592223B (en) | Neodymium-iron-boron magnet galvanization and surface lubrication process | |
| CN104404441A (en) | Preparation method for copper-plated steel band | |
| CN106356187B (en) | Ooze dysprosium technique in a kind of neodymium iron boron surface | |
| CN105112950A (en) | Copper electroplating process | |
| CN112725751B (en) | Preparation method of surface protective coating of ultrathin neodymium-iron-boron permanent magnet | |
| CN103695876A (en) | Process for chemically plating high-performance non-porous nickel-phosphorus alloy | |
| CN104419958A (en) | Neodymium iron boron permanent magnet material low magnetic reducing electroplating method | |
| CN111826688B (en) | Electroplating method of samarium-cobalt magnetic steel |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200410 |