CN110983395A - Magnet, preparation method and wearable device - Google Patents
Magnet, preparation method and wearable device Download PDFInfo
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- CN110983395A CN110983395A CN201911296953.6A CN201911296953A CN110983395A CN 110983395 A CN110983395 A CN 110983395A CN 201911296953 A CN201911296953 A CN 201911296953A CN 110983395 A CN110983395 A CN 110983395A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/02—Processes for applying liquids or other fluent materials performed by spraying
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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
- 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
-
- 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
- C23C14/24—Vacuum evaporation
- C23C14/32—Vacuum evaporation by explosion; by evaporation and subsequent ionisation of the vapours, e.g. ion-plating
-
- 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
-
- 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
Abstract
The invention provides a magnet, a preparation method and wearable equipment, wherein the magnet comprises a magnet body and a first anti-corrosion layer arranged on the surface of the magnet body, the first anti-corrosion layer comprises any one or the combination of at least two of a chemical nickel layer, a passivation metal layer and a corrosion-resistant plastic layer, and the nano oily hole sealing is increased through post-treatment. The magnet realizes the corrosion prevention and rust prevention effects for a longer time, and widens the application range of the magnet.
Description
Technical Field
The invention belongs to the technical field of metal corrosion prevention, and relates to a magnet, a preparation method and wearable equipment.
Background
In recent years, the application and development of the rare earth neodymium iron boron permanent magnet are very rapid, but the neodymium iron boron permanent magnet has poor corrosion resistance and is very easy to corrode in a humid environment. Once corrosion occurs, the magnetic properties of the magnet are degraded, thereby reducing the reliability and stability of the product. Therefore, the application premise of the neodymium iron boron material is to solve the problem of corrosion resistance of the neodymium iron boron material.
At present, the main anticorrosion methods of neodymium iron boron materials include electroplating, phosphating, electrophoresis and the like. Electroplating is used as an anticorrosion method for most neodymium iron boron materials due to its advantages of strong protection capability and stable process. The conventional neodymium iron boron electroplating process is an electroplating nickel copper nickel (Ni-Cu-Ni) process, namely, firstly, a layer of nickel is pre-plated on the surface of a neodymium iron boron material, then, copper is plated on an intermediate layer, and finally, dark nickel and bright nickel are electroplated on the surface layer. However, the corrosion-proof effect is still to be further improved, for example, the magnet of the existing watch is placed outside, and after a period of time, the magnet is corroded and rusted due to sweat and high humidity scenes during wearing.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide the magnet, the preparation method and the wearable equipment, wherein the magnet realizes the corrosion prevention and rust prevention effect for a longer time, and the application range of the magnet is widened.
In order to achieve the purpose, the invention adopts the following technical scheme:
one of the objects of the present invention is to provide a magnet comprising a magnet body and a first corrosion-resistant layer provided on a surface of the magnet body, the first corrosion-resistant layer comprising any one of or a combination of at least two of a chemical nickel layer, a passivated metal layer and a corrosion-resistant plastic layer.
The first anti-corrosion layer can be a separate chemical nickel layer, a passivated metal layer or a corrosion resistant plastic layer; or a combination of a chemical nickel layer and a passivated metal layer or a corrosion resistant plastic layer; or, a combination of a passivated metal layer and a corrosion resistant plastic layer; or, a combination of a chemical nickel layer, a passivated metal layer, and a corrosion resistant plastic layer; the sequence of the chemical nickel layer, the passivation metal layer and the corrosion-resistant plastic layer can be determined according to actual needs.
The magnet is provided with the first anti-corrosion layer on the surface, so that the anti-corrosion and anti-rust effects are remarkably improved, and salt spray test results show that the anti-corrosion and anti-rust time can be prolonged to more than 96 hours, and can reach 168 hours at most.
The magnet further includes a second corrosion protection layer disposed between the magnet body and the first corrosion protection layer. And meanwhile, the first anti-corrosion layer and the second anti-corrosion layer are arranged, so that the anti-corrosion and anti-rust effects of the magnet can be further improved. Typically, the second corrosion protection layer is a nickel-copper-nickel layer.
The thickness of the first corrosion protection layer can be determined by those skilled in the art according to the actual corrosion and rust protection effect, but is preferably less than 100 micrometers, such as 2 micrometers, 3 micrometers, 8 micrometers, 15 micrometers, 20 micrometers, 50 micrometers, 80 micrometers or 90 micrometers, and further preferably 5 to 10 micrometers.
The purpose of the passivated metal layer is to delay or avoid corrosion and rusting of the magnet, so that any metal capable of achieving the effect can be used as the passivated metal layer, and as a preferred technical scheme, the passivated metal layer is selected from any one or a combination of at least two of a metal chromium layer, a metal rhodium layer and a metal cobalt layer, and the combination of the passivated metal layers can be as follows: a combination of a metal chromium layer and a metal rhodium layer, a combination of a metal rhodium layer and a metal cobalt layer, a combination of a metal chromium layer, a metal rhodium layer and a metal cobalt layer, and the like.
The corrosion-resistant plastic layer is also provided for the purpose of delaying or preventing corrosion and rusting of the magnet, and therefore, plastic layers which can achieve the purpose can be used here, and as a preferred technical scheme, the corrosion-resistant plastic layer comprises an epoxy resin layer.
Preferably, the first anti-corrosion layer comprises a chemical nickel layer, a passivated metal layer and a corrosion-resistant plastic layer in a thickness ratio of 2:1 to 2. Within this thickness ratio range, the first anti-corrosion layer works best, i.e. significantly better than the technical effect of a single layer or other composite layers of the same thickness. The thickness ratio of the chemical nickel layer, the passivation metal layer and the corrosion-resistant plastic layer can be 2:1.2:1.8, 2:1.5:2.0, 2:1.7:1.3 or 2:1.3: 1.9.
Preferably, the sum of the thicknesses of the first and second corrosion protection layers is no greater than 20 microns, such as 15 microns, 17 microns, 18 microns, 19 microns, 19.5 microns, or the like
Preferably, the outer surface of the first corrosion prevention layer is further provided with a paraffin layer for filling the pores in the first corrosion prevention layer and coating the surface of the first corrosion prevention layer, so that the corrosion prevention capability is further enhanced.
The invention also aims to provide a preparation method of the magnet, which comprises the steps of preparing any one or a combination of at least two of a chemical nickel layer, a passivated metal layer or a corrosion-resistant plastic layer on the surface of a magnet body; wherein:
preparing a chemical nickel layer by adopting an electroplating process;
preparing a passivated metal layer by adopting a vacuum ion plating method;
and preparing the corrosion-resistant plastic layer by adopting a plastic spraying method.
Preferably, the preparing the chemical nickel layer by using the electroplating process comprises: electroplating in the chemical plating solution to obtain the chemical nickel layer. The chemical plating solution comprises main nickel salt, a complexing agent, a reducing agent, ammonia water and distilled water, and can be a commercially available commodity.
Preferably, the plating temperature is 65-72 deg.C, such as 66 deg.C, 68 deg.C, 70 deg.C, 71 deg.C or 71.5 deg.C.
Preferably, the electroplating time is 35-45min, such as 38min, 40min or 42 min.
Preferably, the plating source of the vacuum ion plating comprises a metal nitride, such as any one of chromium nitride, rhodium nitride or cobalt nitride or a combination of at least two of them, typical but non-limiting combinations include a combination of chromium nitride and rhodium nitride, a combination of rhodium nitride and cobalt nitride, and a combination of chromium nitride, rhodium nitride and cobalt nitride.
Preferably, the pressure of the vacuum ion plating is 0.01 to 135pa, such as 0.05pa, 0.1pa, 0.5pa, 1.0pa, 10pa, 30pa, 50pa, 80pa, 100pa, 120pa, 130.5pa, or the like.
Preferably, the temperature of the vacuum ion plating is 230-280 ℃, such as 235 ℃, 238 ℃, 240 ℃, 255.5 ℃, 260 ℃, 270 ℃ or 275 ℃, and the like.
Preferably, the time of the vacuum ion plating is 110-130min, such as 112min, 115min, 118min, 120min, 125min or 128 min.
Preferably, the spray molding is selected from the group consisting of tumble spraying.
Preferably, the temperature of the plastic spraying is 20-30 ℃, such as 22 ℃, 23 ℃, 25 ℃, 27 ℃ or 29.8 ℃ and the like.
Preferably, the humidity of the spray is 65-85RH, such as 68RH, 70RH, 75RH, 78RH or 82.5 RH.
Preferably, the time for the plastic spraying is 110-.
Preferably, the plastic spraying speed is 3-5r/min, such as 3.5r/min, 4.0r/min, 4.8r/min or 4.8 r/min.
Preferably, paraffin coating is further performed after preparing any one or a combination of at least two of a chemical nickel layer, a passivated metal layer or a corrosion-resistant plastic layer on the surface of the magnet body.
As a preferred technical solution, the preparation method further comprises: preparing a second anti-corrosion layer on the surface of the magnet body, and preparing any one or a combination of at least two of a chemical nickel layer, a passivation metal layer or an anti-corrosion plastic layer on the surface of the second anti-corrosion layer.
The second anti-corrosion layer is selected from a nickel-copper-nickel layer, and the preparation method of the nickel-copper-nickel layer comprises the following steps:
(1) plating bottom nickel: electroplating nickel on a magnet in an electrolyte, wherein the electrolyte contains 260-300g/L nickel sulfate, 45-55g/L nickel chloride and 45-55g/L boric acid, the electroplating temperature is 40-60 ℃, the time is 70-110 minutes, the current is 25-35A, and after the electroplating is finished, the magnet is cleaned and activated by using dilute sulfuric acid with the mass percentage of 1-3%, and then cleaned by using water for 2-5 times;
(2) copper plating: electroplating copper on the nickel-electroplated magnet in an electrolyte, wherein the electrolyte contains 280-320g/L copper pyrophosphate and 60-70g/L potassium pyrophosphate, the electroplating temperature is 45-55 ℃, the electroplating time is 110-130 minutes, the current is 15-25A, and the magnet is cleaned for 2-5 times by using clean water after electroplating;
(3) bright nickel plating: plating bright nickel on the magnet after copper plating in an electrolyte, wherein the electrolyte contains 280-320g/L nickel sulfate, 40-60g/L nickel chloride and 45-55g/L boric acid, the plating temperature is 40-60 ℃, the plating time is 80-100 minutes, the current is 15-25A, and the magnet is washed for 2-5 times by using clear water after plating;
(4) and dehydrating and drying the magnet after the bright nickel plating to obtain the magnet plated with the nickel-copper nickel layer.
Preferably, the magnet body is subjected to a pretreatment including grinding and cleaning prior to the preparation of the second anti-corrosion layer. Grinding the magnet into particles is beneficial to the close attachment of the coating film and the magnet. The pretreatment comprises the steps of cleaning the magnet for 2-5 times by using dilute nitric acid with the mass percentage of 2-5%, then soaking the magnet in hydrofluoric acid with the mass percentage of 8-12%, then immediately taking out the magnet, and then carrying out ultrasonic cleaning.
It is a further object of the present invention to provide a wearable device comprising a magnet as described above. The wearable device includes, but is not limited to, a watch.
Compared with the prior art, the invention has the beneficial effects that:
the magnet provided by the invention realizes the corrosion prevention and rust prevention effects for a longer time, and widens the application range of the magnet.
The preparation method of the magnet provided by the invention is simple and effective, and compared with the magnet obtained by other preparation processes, the magnet has good anti-corrosion and anti-rust effects, and the maximum anti-corrosion time is more than 168 h.
Compared with the prior art, the wearable equipment containing the magnet has better anticorrosive and antirust effects.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Example 1
A magnet comprises a magnet body, and a second anti-corrosion layer and a first anti-corrosion layer which are sequentially arranged on the surface of the magnet body, wherein the second anti-corrosion layer is a nickel-copper nickel layer, and the first anti-corrosion layer is a chemical nickel layer, a metal chromium layer and an epoxy resin layer which are sequentially arranged on the surface of the nickel-copper nickel layer and have a thickness ratio of 2:1.5: 1.5; the thickness of the first anti-corrosion layer is 6 microns; the thickness of the second anti-corrosion layer is 12 microns;
the preparation method of the magnet comprises the following steps:
(1) grinding; grinding the magnet into particles;
(2) pretreatment: cleaning a magnet for 3 times by using dilute nitric acid with the mass percentage of 3%, then soaking the magnet in hydrofluoric acid with the mass percentage of 10%, immediately taking out the magnet, and then performing ultrasonic cleaning to obtain a treated magnet;
(3) plating bottom nickel: electroplating nickel on a magnet in electrolyte, wherein the electrolyte contains 280g/L of nickel sulfate, 50g/L of nickel chloride and 50g/L of boric acid, the electroplating temperature is 50 ℃, the time is 90 minutes, the current is 30A, after the electroplating is finished, cleaning and activating by using dilute sulfuric acid with the mass percentage of 2%, and then cleaning by using water for 3 times;
(4) copper plating: electroplating copper on the nickel-electroplated magnet in electrolyte, wherein the electrolyte contains 300g/L of copper pyrophosphate and 65g/L of potassium pyrophosphate, the electroplating temperature is 50 ℃, the electroplating time is 120 minutes, the current is 20A, and the magnet is cleaned for 3 times by using clean water after being electroplated;
(5) bright nickel plating: plating bright nickel on the magnet after copper plating in electrolyte, wherein the electrolyte contains 300g/L nickel sulfate, 50g/L nickel chloride and 50g/L boric acid, the plating temperature is 50 ℃, the plating time is 90 minutes, the current is 20A, and the magnet is washed for 3 times by using clear water after plating;
(6) dehydrating and drying the magnet after being plated with bright nickel to obtain a magnet plated with a nickel-copper nickel layer;
(7) electroplating in high-phosphorus chemical plating solution to obtain a chemical nickel layer; the electroplating temperature is 70 ℃; the electroplating time is 40 min;
(8) preparing a chromium layer by adopting a vacuum ion plating method; the plating source of the vacuum ion plating is chromium nitride CrN; the pressure of the vacuum ion plating is 0.02 pa; the temperature of the vacuum ion plating is 250 ℃; the time of the vacuum ion plating is 120 min;
(9) preparing an epoxy resin layer by adopting a roll spraying method: the temperature of the plastic spraying is 25 ℃; the humidity of the plastic spraying is 70 RH; the plastic spraying time is 120 min; the plastic spraying speed is 4/min;
(10) and coating a paraffin layer on the surface of the epoxy resin layer.
As another additional embodiment, the order of steps (7), (8) and (9) may be changed, i.e. the order may be (8), (9) and (7), or (9), (7) and (8), or (8), (7) and (9).
Example 2
A magnet comprises a magnet body, and a second anti-corrosion layer and a first anti-corrosion layer which are sequentially arranged on the surface of the magnet body, wherein the second anti-corrosion layer is a nickel-copper nickel layer, and the first anti-corrosion layer is a chemical nickel layer, a metal chromium layer and an epoxy resin layer which are sequentially arranged on the surface of the nickel-copper nickel layer and have a thickness ratio of 2:1: 2; the thickness of the first anti-corrosion layer is 5 microns; the thickness of the second anti-corrosion layer is 12 microns;
the preparation method of the magnet comprises the following steps:
(1) grinding; grinding the magnet into particles;
(2) pretreatment: cleaning a magnet for 5 times by using 2% by mass of dilute nitric acid, then soaking the magnet in 8% by mass of hydrofluoric acid, immediately taking out the magnet, and then performing ultrasonic cleaning to obtain a treated magnet;
(3) plating bottom nickel: electroplating nickel on a magnet in electrolyte, wherein the electrolyte contains 300g/L of nickel sulfate, 45g/L of nickel chloride and 55g/L of boric acid, the electroplating temperature is 40 ℃, the time is 110 minutes, the current is 25A, after the electroplating is finished, cleaning and activating by using dilute sulfuric acid with the mass percentage of 3%, and cleaning by using water for 5 times;
(4) copper plating: electroplating copper on the nickel-electroplated magnet in electrolyte, wherein the electrolyte contains 280g/L of copper pyrophosphate and 70g/L of potassium pyrophosphate, the electroplating temperature is 45 ℃, the electroplating time is 130 minutes, the current is 15A, and the magnet is cleaned for 5 times by using clean water after being electroplated;
(5) bright nickel plating: plating bright nickel on the magnet after copper plating in electrolyte, wherein the electrolyte contains 280g/L nickel sulfate, 60g/L nickel chloride and 45g/L boric acid, the plating temperature is 60 ℃, the plating time is 80 minutes, the current is 25A, and the magnet is washed for 2 times by using clear water after plating;
(6) dehydrating and drying the magnet after being plated with bright nickel to obtain a magnet plated with a nickel-copper nickel layer;
(7) electroplating in high-phosphorus chemical plating solution to obtain a chemical nickel layer; the electroplating temperature is 65 ℃; the electroplating time is 35 min;
(8) preparing a metal chromium layer by adopting a vacuum ion plating method; the plating source of the vacuum ion plating is chromium nitride CrN; the pressure of the vacuum ion plating is 135 pa; the temperature of the vacuum ion plating is 230 ℃; the time of the vacuum ion plating is 130 min;
(9) preparing an epoxy resin layer by adopting a roll spraying method: the temperature of the plastic spraying is 20 ℃; the humidity of the plastic spraying is 85 RH; the plastic spraying time is 110 min; the plastic spraying speed is 5 r/min;
(10) and coating a paraffin layer on the surface of the epoxy resin layer.
Example 3
A magnet comprises a magnet body, and a second anti-corrosion layer and a first anti-corrosion layer which are sequentially arranged on the surface of the magnet body, wherein the second anti-corrosion layer is a nickel-copper nickel layer, and the first anti-corrosion layer is a chemical nickel layer, a metal chromium layer and an epoxy resin layer which are sequentially arranged on the surface of the nickel-copper nickel layer and have a thickness ratio of 2:2: 1; the thickness of the first anti-corrosion layer is 8 microns; the thickness of the second anti-corrosion layer is 12 microns;
the preparation method of the magnet comprises the following steps:
(1) grinding; grinding the magnet into particles;
(2) pretreatment: cleaning a magnet for 2 times by using dilute nitric acid with the mass percentage of 5%, then soaking the magnet in hydrofluoric acid with the mass percentage of 12%, immediately taking out the magnet, and then performing ultrasonic cleaning to obtain a treated magnet;
(3) plating bottom nickel: electroplating nickel on a magnet in electrolyte, wherein the electrolyte contains 260g/L of nickel sulfate, 55g/L of nickel chloride and 45g/L of boric acid, the electroplating temperature is 60 ℃, the time is 70 minutes, the current is 35A, after the electroplating is finished, the magnet is cleaned and activated by using dilute sulfuric acid with the mass percentage of 1%, and then cleaned by using water for 5 times;
(4) copper plating: electroplating copper on the nickel-electroplated magnet in electrolyte, wherein the electrolyte contains 320g/L of copper pyrophosphate and 60g/L of potassium pyrophosphate, the electroplating temperature is 55 ℃, the electroplating time is 110 minutes, the current is 25A, and the magnet is cleaned for 2 times by using clean water after being electroplated;
(5) bright nickel plating: plating bright nickel on the magnet after copper plating in electrolyte, wherein the electrolyte contains 320g/L nickel sulfate, 40g/L nickel chloride and 55g/L boric acid, the plating temperature is 40 ℃, the plating time is 100 minutes, the current is 15A, and the magnet is washed for 5 times by using clear water after plating;
(6) dehydrating and drying the magnet after being plated with bright nickel to obtain a magnet plated with a nickel-copper nickel layer;
(7) electroplating in high-phosphorus chemical plating solution to obtain a chemical nickel layer; the electroplating temperature is 70 ℃; the electroplating time is 45 min;
(8) preparing a metal chromium layer by adopting a vacuum ion plating method; the plating source of the vacuum ion plating is chromium nitride CrN; the pressure of the vacuum ion plating is 0.01 pa; the temperature of the vacuum ion plating is 280 ℃; the time of the vacuum ion plating is 110 min;
(9) preparing an epoxy resin layer by adopting a roll spraying method: the temperature of the plastic spraying is 20 ℃; the humidity of the plastic spraying is 65 RH; the plastic spraying time is 130 min; the plastic spraying speed is 3 r/min;
(10) and coating a paraffin layer on the surface of the epoxy resin layer.
Example 4
A magnet comprises a magnet body, and a second anti-corrosion layer and a first anti-corrosion layer which are sequentially arranged on the surface of the magnet body, wherein the second anti-corrosion layer is a nickel-copper nickel layer, and the first anti-corrosion layer is a chemical nickel layer, a metal chromium layer and an epoxy resin layer which are sequentially arranged on the surface of the nickel-copper nickel layer and have a thickness ratio of 2:1: 1.5; the thickness of the first anti-corrosion layer is 6 microns; the thickness of the second anti-corrosion layer is 12 microns;
the preparation method of the magnet comprises the following steps:
(1) grinding; grinding the magnet into particles;
(2) pretreatment: cleaning a magnet for 4 times by using dilute nitric acid with the mass percentage of 4%, then soaking the magnet in hydrofluoric acid with the mass percentage of 10%, immediately taking out the magnet, and then performing ultrasonic cleaning to obtain a treated magnet;
(3) plating bottom nickel: electroplating nickel on a magnet in electrolyte, wherein the electrolyte contains 270g/L nickel sulfate, 52g/L nickel chloride and 50g/L boric acid, the electroplating temperature is 55 ℃, the time is 100 minutes, the current is 32A, after the electroplating is finished, the magnet is cleaned and activated by using dilute sulfuric acid with the mass percentage of 2%, and then cleaned by using water for 5 times;
(4) copper plating: electroplating copper on the nickel-electroplated magnet in electrolyte, wherein the electrolyte contains 310g/L of copper pyrophosphate and 66g/L of potassium pyrophosphate, the electroplating temperature is 52 ℃, the electroplating time is 125 minutes, the current is 22A, and the magnet is cleaned for 3 times by using clean water after being electroplated;
(5) bright nickel plating: plating bright nickel on the magnet after copper plating in electrolyte, wherein the electrolyte contains 310g/L nickel sulfate, 58g/L nickel chloride and 52g/L boric acid, the plating temperature is 58 ℃, the plating time is 95 minutes, the current is 22A, and the magnet is washed for 5 times by using clean water after plating;
(6) dehydrating and drying the magnet after being plated with bright nickel to obtain a magnet plated with a nickel-copper nickel layer;
(7) electroplating in high-phosphorus chemical plating solution to obtain a chemical nickel layer; the electroplating temperature is 72 ℃; the electroplating time is 45 min;
(8) preparing a metal chromium layer by adopting a vacuum ion plating method; the plating source of the vacuum ion plating is chromium nitride CrN; the pressure of the vacuum ion plating is 0.02 pa; the temperature of the vacuum ion plating is 240 ℃; the time of the vacuum ion plating is 110 min;
(9) preparing an epoxy resin layer by adopting a roll spraying method: the temperature of the plastic spraying is 20 ℃; the humidity of the plastic spraying is 66 RH; the plastic spraying time is 110 min; the plastic spraying speed is 3 r/min.
Example 5
A magnet comprises a magnet body, and a second anti-corrosion layer and a first anti-corrosion layer which are sequentially arranged on the surface of the magnet body, wherein the second anti-corrosion layer is a nickel-copper nickel layer, and the first anti-corrosion layer is a chemical nickel layer, a metal chromium layer and an epoxy resin layer which are sequentially arranged on the surface of the nickel-copper nickel layer and have a thickness ratio of 2:1.5: 1.0; the thickness of the first anti-corrosion layer is 6 microns; the thickness of the second anti-corrosion layer is 12 microns;
the preparation method of the magnet comprises the following steps:
(1) grinding; grinding the magnet into particles;
(2) pretreatment: cleaning a magnet for 3 times by using dilute nitric acid with the mass percentage of 3%, then soaking the magnet in hydrofluoric acid with the mass percentage of 10%, immediately taking out the magnet, and then performing ultrasonic cleaning to obtain a treated magnet;
(3) plating bottom nickel: electroplating nickel on a magnet in electrolyte, wherein the electrolyte contains 280g/L of nickel sulfate, 50g/L of nickel chloride and 50g/L of boric acid, the electroplating temperature is 50 ℃, the time is 90 minutes, the current is 30A, after the electroplating is finished, cleaning and activating by using dilute sulfuric acid with the mass percentage of 2%, and then cleaning by using water for 3 times;
(4) copper plating: electroplating copper on the nickel-electroplated magnet in electrolyte, wherein the electrolyte contains 300g/L of copper pyrophosphate and 65g/L of potassium pyrophosphate, the electroplating temperature is 50 ℃, the electroplating time is 120 minutes, the current is 20A, and the magnet is cleaned for 3 times by using clean water after being electroplated;
(5) bright nickel plating: plating bright nickel on the magnet after copper plating in electrolyte, wherein the electrolyte contains 300g/L nickel sulfate, 50g/L nickel chloride and 50g/L boric acid, the plating temperature is 50 ℃, the plating time is 90 minutes, the current is 20A, and the magnet is washed for 3 times by using clear water after plating;
(6) dehydrating and drying the magnet after being plated with bright nickel to obtain a magnet plated with a nickel-copper nickel layer;
(7) electroplating in high-phosphorus chemical plating solution to obtain a chemical nickel layer; the electroplating temperature is 68 ℃; the electroplating time is 40 min;
(8) preparing a metal chromium layer by adopting a vacuum ion plating method; the plating source of the vacuum ion plating is chromium nitride CrN; the pressure of the vacuum ion plating is 0.03 pa; the temperature of the vacuum ion plating is 270 ℃; the time of the vacuum ion plating is 130 min;
(9) preparing an epoxy resin layer by adopting a roll spraying method: the temperature of the plastic spraying is 22 ℃; the humidity of the plastic spraying is 66 RH; the plastic spraying time is 115 min; the plastic spraying speed is 4 r/min.
Example 6
A magnet comprises a magnet body, and a second anti-corrosion layer and a first anti-corrosion layer which are sequentially arranged on the surface of the magnet body, wherein the second anti-corrosion layer is a nickel-copper nickel layer, and the first anti-corrosion layer is a chemical nickel layer arranged on the surface of the nickel-copper nickel layer; the thickness of the first anti-corrosion layer is 6 microns; the thickness of the second anti-corrosion layer is 12 microns;
the preparation method of the magnet comprises the following steps:
(1) grinding; grinding the magnet into particles;
(2) pretreatment: cleaning a magnet for 3 times by using dilute nitric acid with the mass percentage of 3%, then soaking the magnet in hydrofluoric acid with the mass percentage of 10%, immediately taking out the magnet, and then performing ultrasonic cleaning to obtain a treated magnet;
(3) plating bottom nickel: electroplating nickel on a magnet in electrolyte, wherein the electrolyte contains 280g/L of nickel sulfate, 50g/L of nickel chloride and 50g/L of boric acid, the electroplating temperature is 50 ℃, the time is 90 minutes, the current is 30A, after the electroplating is finished, cleaning and activating by using dilute sulfuric acid with the mass percentage of 2%, and then cleaning by using water for 3 times;
(4) copper plating: electroplating copper on the nickel-electroplated magnet in electrolyte, wherein the electrolyte contains 300g/L of copper pyrophosphate and 65g/L of potassium pyrophosphate, the electroplating temperature is 50 ℃, the electroplating time is 120 minutes, the current is 20A, and the magnet is cleaned for 3 times by using clean water after being electroplated;
(5) bright nickel plating: plating bright nickel on the magnet after copper plating in electrolyte, wherein the electrolyte contains 300g/L nickel sulfate, 50g/L nickel chloride and 50g/L boric acid, the plating temperature is 50 ℃, the plating time is 90 minutes, the current is 20A, and the magnet is washed for 3 times by using clear water after plating;
(6) dehydrating and drying the magnet after being plated with bright nickel to obtain a magnet plated with a nickel-copper nickel layer;
(7) electroplating in high-phosphorus chemical plating solution to obtain a chemical nickel layer; the electroplating temperature is 65 ℃; the time of electroplating is 45 min.
Example 7
A magnet comprises a magnet body, and a second anti-corrosion layer and a first anti-corrosion layer which are sequentially arranged on the surface of the magnet body, wherein the second anti-corrosion layer is a nickel-copper nickel layer, and the first anti-corrosion layer is a metal chromium layer arranged on the surface of the nickel-copper nickel layer; the thickness of the first anti-corrosion layer is 6 microns; the thickness of the second anti-corrosion layer is 12 microns;
the preparation method of the magnet comprises the following steps:
(1) grinding; grinding the magnet into particles;
(2) pretreatment: cleaning a magnet for 3 times by using dilute nitric acid with the mass percentage of 3%, then soaking the magnet in hydrofluoric acid with the mass percentage of 10%, immediately taking out the magnet, and then performing ultrasonic cleaning to obtain a treated magnet;
(3) plating bottom nickel: electroplating nickel on a magnet in electrolyte, wherein the electrolyte contains 280g/L of nickel sulfate, 50g/L of nickel chloride and 50g/L of boric acid, the electroplating temperature is 50 ℃, the time is 90 minutes, the current is 30A, after the electroplating is finished, cleaning and activating by using dilute sulfuric acid with the mass percentage of 2%, and then cleaning by using water for 3 times;
(4) copper plating: electroplating copper on the nickel-electroplated magnet in electrolyte, wherein the electrolyte contains 300g/L of copper pyrophosphate and 65g/L of potassium pyrophosphate, the electroplating temperature is 50 ℃, the electroplating time is 120 minutes, the current is 20A, and the magnet is cleaned for 3 times by using clean water after being electroplated;
(5) bright nickel plating: plating bright nickel on the magnet after copper plating in electrolyte, wherein the electrolyte contains 300g/L nickel sulfate, 50g/L nickel chloride and 50g/L boric acid, the plating temperature is 50 ℃, the plating time is 90 minutes, the current is 20A, and the magnet is washed for 3 times by using clear water after plating;
(6) dehydrating and drying the magnet after being plated with bright nickel to obtain a magnet plated with a nickel-copper nickel layer;
(7) preparing a metal chromium layer by adopting a vacuum ion plating method; the plating source of the vacuum ion plating is chromium nitride CrN; the pressure of the vacuum ion plating is 0.02 pa; the temperature of the vacuum ion plating is 280 ℃; the time of the vacuum ion plating is 130 min.
Example 8
A magnet comprises a magnet body, and a second anti-corrosion layer and a first anti-corrosion layer which are sequentially arranged on the surface of the magnet body, wherein the second anti-corrosion layer is a nickel-copper nickel layer, and the first anti-corrosion layer is an epoxy resin layer arranged on the surface of the nickel-copper nickel layer; the thickness of the first anti-corrosion layer is 6 microns; the thickness of the second anti-corrosion layer is 12 microns;
the preparation method of the magnet comprises the following steps:
(1) grinding; grinding the magnet into particles;
(2) pretreatment: cleaning a magnet for 3 times by using dilute nitric acid with the mass percentage of 3%, then soaking the magnet in hydrofluoric acid with the mass percentage of 10%, immediately taking out the magnet, and then performing ultrasonic cleaning to obtain a treated magnet;
(3) plating bottom nickel: electroplating nickel on a magnet in electrolyte, wherein the electrolyte contains 280g/L of nickel sulfate, 50g/L of nickel chloride and 50g/L of boric acid, the electroplating temperature is 50 ℃, the time is 90 minutes, the current is 30A, after the electroplating is finished, cleaning and activating by using dilute sulfuric acid with the mass percentage of 2%, and then cleaning by using water for 3 times;
(4) copper plating: electroplating copper on the nickel-electroplated magnet in electrolyte, wherein the electrolyte contains 300g/L of copper pyrophosphate and 65g/L of potassium pyrophosphate, the electroplating temperature is 50 ℃, the electroplating time is 120 minutes, the current is 20A, and the magnet is cleaned for 3 times by using clean water after being electroplated;
(5) bright nickel plating: plating bright nickel on the magnet after copper plating in electrolyte, wherein the electrolyte contains 300g/L nickel sulfate, 50g/L nickel chloride and 50g/L boric acid, the plating temperature is 50 ℃, the plating time is 90 minutes, the current is 20A, and the magnet is washed for 3 times by using clear water after plating;
(6) dehydrating and drying the magnet after being plated with bright nickel to obtain a magnet plated with a nickel-copper nickel layer;
(9) preparing an epoxy resin layer by adopting a roll spraying method: the temperature of the plastic spraying is 30 ℃; the humidity of the plastic spraying is 85 RH; the plastic spraying time is 130 min; the plastic spraying speed is 5 r/min.
Example 9
The utility model provides a magnet, magnet includes the magnet body and sets gradually second anticorrosion layer and the first anticorrosion layer on magnet body surface, and the second anticorrosion layer is the nickel copper nickel layer, and first anticorrosion layer is 2.0 for setting up the thickness ratio that sets gradually on nickel copper nickel layer surface: 2.0 of chemical nickel layer and metallic chromium layer; the thickness of the first corrosion protection layer was 6 microns; the thickness of the second anti-corrosion layer is 12 microns;
the preparation method of the magnet comprises the following steps:
(1) obtaining a magnet plated with a nickel-copper-nickel layer according to the method of example 1;
(2) electroplating in high-phosphorus chemical plating solution to obtain a chemical nickel layer; the electroplating temperature is 70 ℃; the electroplating time is 45 min;
(8) preparing a metal chromium layer by adopting a vacuum ion plating method; the plating source of the vacuum ion plating is chromium nitride CrN; the pressure of the vacuum ion plating is 135 pa; the temperature of the vacuum ion plating is 230 ℃; the time of the vacuum ion plating is 130 min.
Example 10
The utility model provides a magnet, magnet includes the magnet body and sets gradually second anticorrosion layer and the first anticorrosion layer on magnet body surface, and the second anticorrosion layer is the nickel copper nickel layer, and first anticorrosion layer is 2.0 for setting up the thickness ratio that sets gradually on nickel copper nickel layer surface: 2.0 layers of chemical nickel and epoxy resin; the thickness of the first corrosion protection layer is 6 microns; the thickness of the second anti-corrosion layer is 12 microns;
the preparation method of the magnet comprises the following steps:
(1) obtaining a magnet plated with a nickel-copper-nickel layer according to the method of example 1;
(2) electroplating in high-phosphorus chemical plating solution to obtain a chemical nickel layer; the electroplating temperature is 70 ℃; the electroplating time is 45 min;
(3) preparing an epoxy resin layer by adopting a roll spraying method: the temperature of the plastic spraying is 20 ℃; the humidity of the plastic spraying is 85 RH; the plastic spraying time is 110 min; the plastic spraying speed is 5 r/min.
Example 11
The utility model provides a magnet, magnet includes the magnet body and sets gradually second anticorrosion layer and the first anticorrosion layer on magnet body surface, and the second anticorrosion layer is the nickel copper nickel layer, and first anticorrosion layer is 2.0 for setting up the thickness ratio that sets gradually on nickel copper nickel layer surface: 2.0 layers of metallic chromium and epoxy resin; the thickness of the first anti-corrosion layer is 6 microns; the thickness of the second anti-corrosion layer is 12 microns;
the preparation method of the magnet comprises the following steps:
(1) obtaining a magnet plated with a nickel-copper-nickel layer according to the method of example 1;
(2) preparing a metal chromium layer by adopting a vacuum ion plating method; the plating source of the vacuum ion plating is chromium nitride CrN; the pressure of the vacuum ion plating is 0.01 pa; the temperature of the vacuum ion plating is 280 ℃; the time of the vacuum ion plating is 110 min;
(3) preparing an epoxy resin layer by adopting a roll spraying method: the temperature of the plastic spraying is 20 ℃; the humidity of the plastic spraying is 85 RH; the plastic spraying time is 110 min; the plastic spraying speed is 5 r/min.
Example 12
A wristwatch comprising the magnet according to any one of embodiments 1-1.
Comparative example 1
A magnet as the ground granular magnet body of example 1.
Comparative example 2
A magnet comprises a magnet body and a second anti-corrosion layer arranged on the surface of the magnet body, wherein the second anti-corrosion layer is a nickel-copper-nickel layer, and the thickness of the second anti-corrosion layer is 12 microns;
the magnet is plated with a nickel-copper-nickel layer by the method of the embodiment 1;
comparative example 3
A magnet comprises a magnet body, and a second anti-corrosion layer and a first anti-corrosion layer which are sequentially arranged on the surface of the magnet body, wherein the second anti-corrosion layer is a nickel-copper nickel layer, and the first anti-corrosion layer is a chemical nickel layer, a metal chromium layer and an epoxy resin layer which are sequentially arranged on the surface of the nickel-copper nickel layer and have a thickness ratio of 2:1.5: 2.0;
the preparation method of the magnet comprises the following steps:
(1) obtaining a magnet plated with a nickel-copper-nickel layer according to the method of example 1;
(2) electroplating in high-phosphorus chemical plating solution to obtain a chemical nickel layer; the electroplating temperature is 65 ℃; the electroplating time is 30 min;
(3) preparing a metal chromium layer by adopting a vacuum ion plating method; the plating source of the vacuum ion plating is chromium nitride CrN; the pressure of the vacuum ion plating is 0.005 pa; the temperature of the vacuum ion plating is 225 ℃; the time of the vacuum ion plating is 105 min;
(4) preparing an epoxy resin layer by adopting a roll spraying method: the temperature of the plastic spraying is 18 ℃; the humidity of the plastic spraying is 60 RH; the plastic spraying time is 105 min; the plastic spraying speed is 2 r/min.
Comparative example 4
A magnet comprises a magnet body, and a second anti-corrosion layer and a first anti-corrosion layer which are sequentially arranged on the surface of the magnet body, wherein the second anti-corrosion layer is a nickel-copper nickel layer, and the first anti-corrosion layer is a chemical nickel layer, a metal chromium layer and an epoxy resin layer which are sequentially arranged on the surface of the nickel-copper nickel layer and have a thickness ratio of 1:1.5: 2.0;
the preparation method of the magnet comprises the following steps:
(1) obtaining a magnet plated with a nickel-copper-nickel layer according to the method of example 1;
(2) electroplating in high-phosphorus chemical plating solution to obtain a chemical nickel layer; the electroplating temperature is 88 ℃; the electroplating time is 50 min;
(3) preparing a metal chromium layer by adopting a vacuum ion plating method; the plating source of the vacuum ion plating is chromium nitride CrN; the pressure of the vacuum ion plating is 140 pa; the temperature of the vacuum ion plating is 285 ℃; the time of the vacuum ion plating is 135 min;
(4) preparing an epoxy resin layer by adopting a roll spraying method: the temperature of the plastic spraying is 35 ℃; the humidity of the plastic spraying is 88 RH; the plastic spraying time is 135 min; the plastic spraying speed is 6 r/min.
The corrosion prevention effects of examples 1 to 11 and comparative examples 1 to 3 were tested by the salt spray test (the salt spray standard was referred to the NSS standard), and the results showed that the corrosion resistance times of the magnets obtained in examples 1 to 11 were all greater than 72 hours, and the corrosion resistance times of the magnets obtained in examples 1 to 5 were greater than 96 hours, wherein the corrosion resistance times of the magnets obtained in examples 1 to 3 were greater than 168 hours. Whereas the corrosion prevention time of the magnets obtained in comparative examples 1 to 4 was up to 72 hours.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are within the scope and disclosure of the present invention.
Claims (10)
1. A magnet, comprising a magnet body and a first corrosion prevention layer provided on a surface of the magnet body, wherein the first corrosion prevention layer comprises any one or a combination of at least two of a chemical nickel layer, a passivated metal layer and a corrosion-resistant plastic layer.
2. The magnet according to claim 1, further comprising a second corrosion protection layer disposed between the magnet body and the first corrosion protection layer.
3. The magnet according to claim 1 or 2, wherein the thickness of the first anticorrosive layer is 5 to 10 μm.
4. The magnet according to any one of claims 1 to 3, wherein the passivation metal layer is selected from any one of a metal chromium layer, a metal rhodium layer or a metal cobalt layer or a combination of at least two of them;
preferably, the sum of the thicknesses of the first and second corrosion protection layers is no greater than 20 microns.
5. The magnet according to any one of claims 1 to 4, wherein the corrosion resistant plastic layer comprises an epoxy resin layer.
6. The magnet according to any one of claims 1 to 5, wherein said first anticorrosive layer comprises a chemical nickel layer, a passivated metal layer and a corrosion-resistant plastic layer in a thickness ratio of 2:1 to 2;
preferably, the outer surface of the first anti-corrosion layer is also provided with a paraffin layer.
7. The method for producing a magnet according to any one of claims 1 to 6, comprising producing any one of or a combination of at least two of a chemical nickel layer, a passivated metal layer, or a corrosion-resistant plastic layer on the surface of the magnet body; wherein:
preparing a chemical nickel layer by adopting an electroplating process;
preparing a passivated metal layer by adopting a vacuum ion plating method;
and preparing the corrosion-resistant plastic layer by adopting a plastic spraying method.
8. The method for preparing the nickel alloy sheet according to the claim 7, wherein the step of preparing the chemical nickel layer by using the electroplating process comprises the following steps: electroplating in chemical plating solution to obtain a chemical nickel layer;
preferably, the temperature of the electroplating is 65-72 ℃;
preferably, the electroplating time is 35-45 min;
preferably, the plating source of the vacuum ion plating includes a metal nitride;
preferably, the pressure of the vacuum ion plating is 0.01-135 pa;
preferably, the temperature of the vacuum ion plating is 230-280 ℃;
preferably, the time of the vacuum ion plating is 110-130 min;
preferably, the plastic spraying is selected from the group consisting of tumble spraying;
preferably, the temperature of the plastic spraying is 20-30 ℃;
preferably, the humidity of the plastic spraying is 65-85 RH;
preferably, the time for plastic spraying is 110-;
preferably, the speed of the plastic spraying is 3-5 r/min;
preferably, paraffin coating is further performed after preparing any one or a combination of at least two of a chemical nickel layer, a passivated metal layer or a corrosion-resistant plastic layer on the surface of the magnet body.
9. The production method according to claim 7 or 8, wherein a second anticorrosive layer is produced on the surface of the magnet body, and then any one or a combination of at least two of a chemical nickel layer, a passivated metal layer or an anticorrosive plastic layer is produced on the surface of the second anticorrosive layer;
preferably, the magnet body is subjected to a pretreatment including grinding and cleaning prior to the preparation of the second anti-corrosion layer.
10. A wearable device comprising the magnet of any of claims 1-6.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112289538A (en) * | 2020-12-22 | 2021-01-29 | 安费诺定制连接器(常州)有限公司 | Corrosion-resistant and wear-resistant magnet and treatment method thereof |
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