Composite electroplating method for sintered Nd—Fe-B magnet
11242612 · 2022-02-08
Assignee
- NINGBO YUNSHENG CO., LTD. (Zhejiang, CN)
- NINGBO YUNSHENG MAGNET DEVICES TECHNOLOGY CO., LTD. (Zhejiang, CN)
Inventors
Cpc classification
C25D5/605
CHEMISTRY; METALLURGY
C25D5/12
CHEMISTRY; METALLURGY
C25D5/34
CHEMISTRY; METALLURGY
C25D5/14
CHEMISTRY; METALLURGY
International classification
C25D5/14
CHEMISTRY; METALLURGY
C25D7/00
CHEMISTRY; METALLURGY
C25D5/00
CHEMISTRY; METALLURGY
C25D5/34
CHEMISTRY; METALLURGY
C25D5/12
CHEMISTRY; METALLURGY
Abstract
Disclosed is a composite electroplating method for sintered NdFeB magnet, including: a process of pre-treating sintered NdFeB magnet, a process of electroplating the pre-treated sintered NdFeB magnet, and a process of cleaning and drying the electroplated sintered NdFeB magnet. The electroplating process forms a composite coating composed of a Zn coating, a Zn—Ni alloy coating, a Cu coating and a Ni coating on the surface of the sintered NdFeB magnet.
Claims
1. A composite electroplating method for sintered NdFeB magnet, comprising: {circle around (1)} a process of pre-treating a sintered NdFeB magnet, {circle around (2)} a process of electroplating the pre-treated sintered NdFeB magnet, and {circle around (3)} a process of cleaning and drying the electroplated sintered NdFeB magnet, wherein the process of electroplating the pre-treated sintered NdFeB magnet comprises the following steps: {circle around (2)}-1 performing an electro-galvanizing treatment on the pre-treated sintered NdFeB magnet to form a Zn coating on the surface of the sintered NdFeB magnet; {circle around (2)}-2 performing a first activation treatment on the electro-galvanized sintered NdFeB magnet; {circle around (2)}-3 performing a Zn—Ni alloy electroplating treatment on the sintered NdFeB magnet after the first activation treatment to form a Zn—Ni alloy coating on the surface of the Zn coating; {circle around (2)}-4 performing a second activation treatment on the sintered NdFeB magnet after the Zn—Ni alloy electroplating treatment; {circle around (2)}-5 performing a Cu electroplating treatment on the sintered NdFeB magnet after the second activation treatment to form a Cu coating on the surface of the Zn—Ni alloy coating; and {circle around (2)}-6 performing a Ni electroplating treatment on the sintered NdFeB magnet after the Cu electroplating treatment to form a Ni coating on the surface of the Cu coating, wherein the process of the Zn—Ni alloy electroplating treatment in step {circle around (2)}-3 uses a Zn—Ni allo solution as an electroplating solution; the Zn—Ni alloy solution has a temperature of 30-35° C. and a pH of 5-5.5, and the Zn—Ni alloy solution is formed by uniformly mixing potassium chloride, zinc chloride, nickel chloride and water; every liter of the Zn—Ni alloy solution comprises 150-200 g of potassium chloride, 40-70 g of zinc chloride, and 80-120 g of nickel chloride; the Zn—Ni alloy electroplating treatment is carried out for 1-2.5 h; and the thickness of the Zn—Ni alloy coating is 1.5-4 μm.
2. The composite electroplating method for a sintered NdFeB magnet according to claim 1, wherein the process of the electro-galvanizing treatment in the step {circle around (2)}-1 uses a zinc sulfate solution as an electroplating solution, the zinc sulfate solution has a PH of 4-5 and a temperature of 20-40° C., and the zinc sulfate solution is formed by uniformly mixing zinc sulfate heptahydrate, boric acid, a brightener and water; every liter of the zinc sulfate solution comprises 380-400 g of zinc sulfate heptahydrate, 20 g-40 g of boric acid, and 0.1-0.2 ml of the brightener; the electro-galvanizing treatment is carried out for 1-2 h; and the thickness of the zinc coating is 2-4 μm.
3. The composite electroplating method for sintered NdFeB magnet according to claim 1, wherein the process of the first activation treatment in step {circle around (2)}-2 is as follows: the electro-galvanized sintered NdFeB magnet is activated with a first activating solution for 5-15 s, the first activating solution is formed by uniformly mixing HNO.sub.3, HCl and water, and in the first activating solution, the content of HNO.sub.3 is 5 ml/L and the content of HCl is 5 ml/L.
4. The composite electroplating method for sintered NdFeB magnet according to claim 1, wherein the process of the second activation treatment in step {circle around (2)}-4 is as follows: the sintered NdFeB magnet after the Zn—Ni alloy electroplating treatment is activated with a second activating solution for 10-20 s, the second activating solution is formed by uniformly mixing citric acid and water, and the content of citric acid in the second activating solution is 0.2-0.5 g/L.
5. The composite electroplating method for a sintered NdFeB magnet according to claim 1, wherein the process of the Cu electroplating treatment in step {circle around (2)}-5 uses a Cu solution as an electroplating solution; the Cu solution has a temperature of 45° C. and a PH of 9-12, and the Cu solution is formed by uniformly mixing copper pyrophosphate, potassium pyrophosphate, and water; every liter of the Cu solution comprises 30-70 g of copper pyrophosphate and 240-400 g of potassium pyrophosphate; the Cu electroplating treatment is carried out for 2-4 h; and the thickness of the Cu coating is 3-5 μm.
6. The composite electroplating method for sintered NdFeB magnet according to claim 1, wherein the process of the Ni electroplating treatment in step {circle around (2)}-6 uses a Ni solution as an electroplating solution; the Ni solution has a temperature of 45° C. and a PH of 4, and the Ni solution is formed by uniformly mixing nickel sulfate, nickel chloride, and water; every liter of the Ni solution comprises 250-350 g of nickel sulfate and 30-70 g of nickel chloride; the Ni electroplating treatment is carried out for 2-4 h; and the thickness of the Ni coating is 3-7 μm.
7. The composite electroplating method for sintered NdFeB magnet according to claim 1, wherein the process of pre-treating the sintered NdFeB magnet in the step {circle around (1)} comprises the following steps: {circle around (1)}-1 vibromilling and chamfering the sintered NdFeB magnet; {circle around (1)}-2 dipping and degreasing the vibromilled and chamfered sintered NdFeB magnet for 2-10 min in the presence of a dipping and degreasing solution which has a PH of 9-13 and a temperature of 50-65° C.; {circle around (1)}-3 pickling the dipped and degreased sintered NdFeB magnet for 15-300 s by using a nitric acid solution with a volume concentration of 2-5%; {circle around (1)}-4 ultrasonically cleaning the pickled sintered NdFeB magnet to remove magnetic powder attached to the surface of the-pickled sintered NdFeB magnet, wherein an ultrasonic cleaning solution is formed by uniformly mixing sodium citrate and water, and the mass percentage concentration of sodium citrate in the ultrasonic cleaning solution is 5%; and {circle around (1)}-5 rinsing the ultrasonically cleaned sintered NdFeB magnet for three times with overflow water.
Description
DETAILED DESCRIPTION
(1) With reference to the embodiments, the invention will be described in more details below.
(2) Embodiment 1: A composite electroplating method for a sintered NdFeB magnet, including: {circle around (1)} a process of pre-treating sintered NdFeB magnet, {circle around (2)} a process of electroplating the pre-treated sintered NdFeB magnet, and {circle around (3)} a process of cleaning and drying the electroplated sintered NdFeB magnet; the process of electroplating the pre-treated sintered NdFeB magnet specifically includes the following steps:
(3) {circle around (2)}-1 electro-galvanizing the pre-treated sintered NdFeB magnet to form a Zn coating on the surface of the sintered NdFeB magnet;
(4) {circle around (2)}-2 performing first activation treatment on the electro-galvanized sintered NdFeB magnet;
(5) {circle around (2)}-3 performing Zn—Ni alloy electroplating treatment on the sintered NdFeB magnet after the first activation treatment to form Zn—Ni alloy coating on the surface of the Zn coating;
(6) {circle around (2)}-4 performing second activation treatment on the sintered NdFeB magnet after the Zn—Ni alloy electroplating treatment;
(7) {circle around (2)}-5 performing Cu electroplating treatment on the sintered NdFeB magnet after the second activation treatment to form Cu coating on the surface of the Zn—Ni alloy coating;
(8) {circle around (2)}-6 performing Ni electroplating treatment on the sintered NdFeB magnet after the Cu electroplating treatment to form a Ni coating on the surface of the Cu coating.
(9) Embodiment 2: A composite electroplating method for sintered NdFeB magnet, including {circle around (1)} a process of pre-treating sintered NdFeB magnet, {circle around (2)} a process of electroplating the pre-treated sintered NdFeB magnet, and {circle around (3)} a process of cleaning and drying the electroplated sintered NdFeB magnet; the process of electroplating the pre-treated sintered NdFeB magnet specifically includes the following steps:
(10) {circle around (2)}-1 electro-galvanizing the pre-treated sintered NdFeB magnet to form a Zn coating on the surface of the sintered NdFeB magnet;
(11) {circle around (2)}-2 performing first activation treatment on the electro-galvanized sintered NdFeB magnet;
(12) {circle around (2)}-3 performing Zn—Ni alloy electroplating treatment on the sintered NdFeB magnet after the first activation treatment to form a Zn—Ni alloy coating on the surface of the Zn coating;
(13) {circle around (2)}-4 performing second activation treatment on the sintered NdFeB magnet after the Zn—Ni alloy electroplating treatment;
(14) {circle around (2)}-5 performing Cu electroplating treatment on the sintered NdFeB magnet after the second activation treatment to form a Cu coating on the surface of the Zn—Ni alloy; {circle around (2)}-6 performing Ni electroplating treatment on the sintered NdFeB magnet after the Cu electroplating treatment to form a Ni coating on the surface of the Cu coating.
(15) In this embodiment, the electro-galvanizing process in the step {circle around (2)}-1 uses a zinc sulfate solution as an electroplating solution. The zinc sulfate solution has a PH of 4-5 and a temperature of 40° C., and the zinc sulfate solution is formed by uniformly mixing zinc sulfate heptahydrate, boric acid, a brightener and water. Every liter of the zinc sulfate solution includes 400 g of zinc sulfate heptahydrate, 40 g of boric acid, and 0.2 ml of the brightener. The electro-galvanizing treatment is carried out for 2 h, and the thickness of the zinc coating is 4 μm.
(16) In this embodiment, the specific process of the first activation treatment in step {circle around (2)}-2 is as follows: the electro-galvanized sintered NdFeB magnet is activated with a first activating solution for 15 s, and the first activating solution is formed by uniformly mixing HNO.sub.3, HCl and water. In the first activating solution, the content of HNO.sub.3 is 5 ml/L and the content of HCl is 5 ml/L.
(17) In this embodiment, the Zn—Ni alloy electroplating treatment process in step {circle around (2)}-3 uses a Zn—Ni Ni alloy solution as an electroplating solution. The Zn—Ni alloy solution has a temperature of 35° C. and a PH of 5.5, and the Zn—Ni alloy solution is formed by uniformly mixing potassium chloride, zinc chloride, nickel chloride and water. Every liter of the Zn—Ni alloy solution includes 200 g of potassium chloride, 70 g of zinc chloride, and 120 g of nickel chloride. The Zn—Ni alloy electroplating treatment is carried out for 2.5 h, and the thickness of the Zn—Ni alloy coating is 4 μm.
(18) In this embodiment, the specific process of the second activation treatment in step {circle around (2)}-4 is as follows: the sintered NdFeB magnet after the Zn—Ni alloy electroplating treatment is activated with a second activating solution for 20 s, and the second activating solution is formed by uniformly mixing citric acid and water. The content of citric acid in the second activating solution is 0.5 g/L.
(19) In this embodiment, the Cu electroplating treatment process in step {circle around (2)}-5 uses a Cu solution as an electroplating solution. The Cu solution has a temperature of 45° C. and a PH of 12, and the Cu solution is formed by uniformly mixing copper pyrophosphate, potassium pyrophosphate, and water. Every liter of the Cu solution includes 70 g of copper pyrophosphate and 400 g of potassium pyrophosphate. The Cu electroplating treatment is carried out for 4 h, and the thickness of the Cu coating is 5 μm.
(20) In this embodiment, the Ni electroplating treatment process in step {circle around (2)}-6 uses a Ni solution as an electroplating solution. The Ni solution has a temperature of 45° C. and a PH of 4, and the Ni solution is formed by uniformly mixing nickel sulfate, nickel chloride, and water. Every liter of the Ni solution includes 350 g of nickel sulfate and 70 g of nickel chloride. The Ni electroplating treatment is carried out for 4 h, and the thickness of the Ni coating is 7 μm.
(21) In this embodiment, the pretreatment process for the sintered NdFeB magnet in the step {circumflex over (1)} includes the following steps:
(22) {circle around (1)}-1 vibromilling and chamfering the sintered NdFeB magnet;
(23) {circle around (1)}-2 dipping and degreasing the vibromilled and chamfered sintered NdFeB magnet for 10 min in the presence of a dipping and degreasing solution which has a PH of 13 and a temperature of 65° C.;
(24) {circle around (1)}-3 pickling the dipped and degreased sintered NdFeB magnet for 300 s by using a nitric acid solution with a volume concentration of 5%;
(25) {circle around (1)}-4 ultrasonically cleaning the pickled sintered NdFeB magnet to remove magnetic powder attached to the surface of the product after pickling, wherein an ultrasonic cleaning solution is formed by uniformly mixing sodium citrate and water, and the mass percentage concentration of sodium citrate in the ultrasonic cleaning solution is 5%; and
(26) {circle around (1)}-5 rinsing the ultrasonically cleaned sintered NdFeB magnet for three times with overflow water.
(27) Embodiment 3: A composite electroplating method for sintered NdFeB magnet, including: {circle around (1)} a process of pre-treating sintered NdFeB magnet, {circle around (2)} a process of electroplating the pre-treated sintered NdFeB magnet, and {circle around (3)} a process of cleaning and drying the electroplated sintered NdFeB magnet; the process of electroplating the pre-treated sintered NdFeB magnet specifically includes the following steps:
(28) {circle around (2)}-1 electro-galvanizing the pre-treated sintered NdFeB magnet to form a Zn coating on the surface of the sintered NdFeB magnet;
(29) {circle around (2)}-2 performing first activation treatment on the electro-galvanized sintered NdFeB magnet;
(30) {circle around (2)}-3 performing Zn—Ni alloy electroplating treatment on the sintered NdFeB magnet after the first activation treatment to form a Zn—Ni alloy coating on the surface of the Zn coating;
(31) {circle around (2)}-4 performing second activation treatment on the sintered NdFeB magnet after the Zn—Ni alloy electroplating treatment;
(32) {circle around (2)}-5 performing Cu electroplating treatment on the sintered NdFeB magnet after the second activation treatment to form Cu coating on the surface of the Zn—Ni alloy coating;
(33) {circle around (2)}-6 performing Ni electroplating treatment on the sintered NdFeB magnet after the Cu electroplating treatment to form a Ni coating on the surface of the Cu coating.
(34) In this embodiment, the electro-galvanizing process in the step {circle around (2)}-1 uses a zinc sulfate solution as an electroplating solution. The zinc sulfate solution has a PH of 4 and a temperature of 20° C., and the zinc sulfate solution is formed by uniformly mixing zinc sulfate heptahydrate, boric acid, a brightener and water. Every liter of the zinc sulfate solution includes 380 g of zinc sulfate heptahydrate, 20 g of boric acid, and 0.1 ml of the brightener. The electro-galvanizing treatment is carried out for 1 h, and the thickness of the zinc coating is 2 μm.
(35) In this embodiment, the specific process of the first activation treatment in step {circle around (2)}-2 is as follows: the electro-galvanized sintered NdFeB magnet is activated with a first activating solution for 5 s, and the first activating solution is formed by uniformly mixing HNO.sub.3, HCl and water. In the first activating solution, the content of HNO.sub.3 is 5 ml/L and the content of HCl is 5 ml/L.
(36) In this embodiment, the Zn—Ni alloy electroplating treatment process in step {circle around (2)}-3 uses a Zn—Ni alloy solution as an electroplating solution. The Zn—Ni alloy solution has a temperature of 30° C. and a PH of 5, and the Zn—Ni alloy solution is formed by uniformly mixing potassium chloride, zinc chloride, nickel chloride and water. Every liter of the Zn—Ni alloy solution includes 150 g of potassium chloride, 40 g of zinc chloride, and 80 g of nickel chloride. The Zn—Ni alloy electroplating treatment is carried out for 1 h, and the thickness of the Zn—Ni alloy coating is 1.5 μm.
(37) In this embodiment, the specific process of the second activation treatment in step {circle around (2)}-4 is as follows: the sintered NdFeB magnet after the Zn—Ni alloy electroplating treatment is activated with a second activating solution for 10 s, and the second activating solution is formed by uniformly mixing citric acid and water. The content of citric acid in the second activating solution is 0.2 g/L.
(38) In this embodiment, the Cu electroplating treatment process in step {circle around (2)}-5 uses a Cu solution as an electroplating solution. The Cu solution has a temperature of 45° C. and a PH of 9, and the Cu solution is formed by uniformly mixing copper pyrophosphate, potassium pyrophosphate, and water. Every liter of the Cu solution includes 30 g of copper pyrophosphate and 240 g of potassium pyrophosphate. The Cu electroplating treatment is carried out for 2 h, and the thickness of the Cu coating is 3 μm.
(39) In this embodiment, the Ni electroplating treatment process in step {circle around (2)}-6 uses a Ni solution as an electroplating solution. The Ni solution has a temperature of 45° C. and a PH of 4, and the Ni solution is formed by uniformly mixing nickel sulfate, nickel chloride, and water. Every liter of the Ni solution includes 250 g of nickel sulfate and 30 g of nickel chloride. The Ni electroplating treatment is carried out for 2 h, and the thickness of the Ni coating is 3 μm.
(40) In this embodiment, the pretreatment process for the sintered NdFeB magnet in the step {circle around (1)} includes the following steps:
(41) {circle around (1)}-1 vibromilling and chamfering the sintered NdFeB magnet;
(42) {circle around (1)}-2 dipping and degreasing the vibromilled and chamfered sintered NdFeB for 2 min in the presence of a dipping and degreasing solution which has a PH of 9 and a temperature of 50° C.;
(43) {circle around (1)}-3 pickling the dipped and degreased sintered NdFeB magnet for 15 s by using a nitric acid solution with a volume concentration of 2%;
(44) {circle around (1)}-4 ultrasonically cleaning the pickled sintered NdFeB magnet to remove magnetic powder attached to the surface of the product after pickling, wherein an ultrasonic cleaning solution is formed by uniformly mixing sodium citrate and water, and the mass percentage concentration of sodium citrate in the ultrasonic cleaning solution is 5%;
(45) {circle around (1)}-5 rinsing the ultrasonically cleaned sintered NdFeB magnet for three times with overflow water.