CN112458502A - Electroplating method of ultrathin coating for neodymium iron boron - Google Patents
Electroplating method of ultrathin coating for neodymium iron boron Download PDFInfo
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- CN112458502A CN112458502A CN202011069753.XA CN202011069753A CN112458502A CN 112458502 A CN112458502 A CN 112458502A CN 202011069753 A CN202011069753 A CN 202011069753A CN 112458502 A CN112458502 A CN 112458502A
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- iron boron
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/38—Electroplating: Baths therefor from solutions of copper
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- C—CHEMISTRY; METALLURGY
- 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
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
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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
- 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
Abstract
The invention discloses an electroplating method of an ultrathin coating for neodymium iron boron, which comprises the steps of coating the surface of a neodymium iron boron substrate, namely respectively electroplating a cyanide-free alkali copper coating and a chemical nickel coating from inside to outside; the process for electroplating the cyanide-free alkali copper plating layer adopts a copper plating solution, wherein the chemical components of the copper plating solution comprise copper carbonate, HEDP, potassium carbonate, potassium hydroxide, bismuth nitrate and polycation quaternary ammonium salt; the temperature of the copper plating solution is 40-60 ℃, and the pH value is 9-12. The method can coat a compact cyanide-free alkali copper plating layer and a compact chemical nickel plating layer on the surface of the neodymium iron boron substrate, so that the porosity can be guaranteed under the condition of very thin plating layer thickness, and the substrate is prevented from being corroded.
Description
Technical Field
The invention belongs to the technical field of metal surface treatment, and particularly relates to an electroplating method of an ultrathin coating for neodymium iron boron.
Background
At present, the neodymium iron boron permanent magnet material is used as a magnetic material with high magnetic performance and high cost performance, and is widely applied to a plurality of fields such as electronic machinery, medical equipment and the like. However, because of some characteristics of the ndfeb substrate, such as easy oxidation of the substrate, porous and loose substrate, etc., the surface treatment of the ndfeb substrate has been a difficulty.
At present, NiCuNi plating (the thickness is usually 5-15 μm) and CuEN plating (the thickness is usually 6-8 μm) are relatively stable plating layers on the surface of a neodymium iron boron substrate, but with the increasing requirements of electronic consumer products on the lightness and thinness of products, the low porosity is required to be met by a common copper layer and a chemical nickel layer, the single-layer electroplating needs 4-5 micrometers, the traditional plating scheme is not satisfactory, and a thin plating layer which is non-magnetic shielding and compact is urgently needed.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention aims to provide an electroplating method of an ultrathin plating layer for neodymium iron boron, and a compact cyanide-free alkali copper plating layer and a compact chemical nickel plating layer can be plated on the surface of a neodymium iron boron substrate by the method, so that the porosity can be ensured under the condition of very thin plating layer thickness, and the substrate is prevented from being corroded.
The electroplating method of the ultrathin coating for the neodymium iron boron is characterized in that the surface of a neodymium iron boron substrate is coated, and an electroplating cyanide-free alkali copper coating and a chemical nickel coating are respectively coated from inside to outside;
the process for electroplating the cyanide-free alkali copper plating layer adopts a copper plating solution, wherein the chemical components of the copper plating solution comprise copper carbonate, HEDP, potassium carbonate, potassium hydroxide, bismuth nitrate and polycation quaternary ammonium salt; the temperature of the copper plating solution is 40-60 ℃, and the pH value is 9-12. In the copper plating solutions of the present application, HEDP acts as a complexing agent.
The electroplating method of the ultrathin coating for the neodymium iron boron is characterized in that the mass concentrations of all chemical components in a copper plating solution are as follows:
20-30 g/L of copper carbonate
HEDP 170-220g/L
70-90g/L potassium carbonate
160g/L potassium hydroxide
0.03-0.08g/L bismuth nitrate
0.001-0.005g/L of polycationic quaternary ammonium salt.
The electroplating method of the ultrathin coating for the neodymium iron boron is characterized in that the polycation quaternary ammonium salt is polyquaternium-7, polyquaternium-10 or polyquaternium-22.
The electroplating method of the ultrathin coating for the neodymium iron boron is characterized in that a nickel plating solution is adopted in the chemical nickel coating process, and the chemical components of the nickel plating solution comprise nickel sulfate, sodium hypophosphite, citric acid, malic acid, sodium hydroxide, PPS-OH and allyl iodide; the temperature of the nickel plating solution is 75-90 ℃, and the pH value is 4.6-5.0.
In the nickel plating solution of the present application, sodium hypophosphite acts as a reducing agent, citric acid and malic acid both act as complexing agents, and allyl iodide acts as a stabilizer.
The electroplating method of the ultrathin coating for the neodymium iron boron is characterized in that the mass concentrations of all chemical components in the nickel plating solution are as follows:
nickel sulfate 20-25g/L
18-23g/L sodium hypophosphite
Citric acid 10-15g/L
Malic acid 8-12g/L
16-24g/L of sodium hydroxide
PPS-OH 0.005-0.01g/L
Allyl iodide 0.002-0.007 g/L.
The electroplating method of the ultrathin coating for the neodymium iron boron is characterized in that the thickness of the cyanide-free alkali copper coating is 2-4 mu m, and the thickness of the chemical nickel coating is 1-2 mu m.
The electroplating method of the ultrathin coating for the neodymium iron boron is characterized by comprising the following steps:
1) carrying out oil removal, acid washing and activation treatment on the neodymium iron boron substrate before plating;
2) placing the pretreated neodymium iron boron base material into a copper plating solution, and electroplating under the action of current to obtain a cyanide-free alkali copper plating layer on the surface of the neodymium iron boron base material; wherein the current density adopted during electroplating is 0.1-0.5 ASD, and the electroplating time is 60-120 minutes;
3) after the cyanide-free alkali copper plating layer is electroplated, putting the neodymium iron boron base material into a nickel plating solution for chemical nickel plating to obtain a neodymium iron boron material after chemical nickel plating; wherein the temperature for chemical nickel plating is 75-90 ℃ and the time is 40-80 minutes.
Compared with the prior art, the technical effect that this application gained is:
1. the polycation quaternary ammonium salt is initiatively added into the copper plating solution, contains electron-deficient groups, the higher the current density is, the more electrons are released by a cathode, the more the polycation quaternary ammonium salt is adsorbed at the position, and the function of shielding high current is achieved, so that more copper can be deposited at the position of low current density and a substrate pit, and a compact electroplated copper layer can be formed only by electroplating 2-4 microns; the polycation quaternary ammonium salt can play a role of a deep-plating agent.
2. In the conventional nickel plating process, the sodium hypochlorite can release electrons under the catalysis of a nickel layer, and the released electrons are captured by nickel ions, so that the nickel ions are reduced into nickel metal to be deposited on the surface of a base material. In the invention, PPS-OH contained in the adopted nickel plating solution can be adsorbed on the surface of a product, and the PPS-OH contains pyridinium salt which can compete with nickel ions to capture electrons, so that the nickel ions delay the electron deposition, the nickel atom micro-deposition mode is changed, the chemical nickel plating layer is more densely stacked, and the compact chemical nickel plating layer can be formed only by electroplating 1-2 microns.
Drawings
FIG. 1 shows the results of metallographic measurements carried out on sample A prepared in example 1;
FIG. 2 shows the results of metallographic tests carried out on sample B prepared in example 2;
FIG. 3 is the result of metallographic test on sample C prepared in comparative example 1;
FIG. 4 is a photograph comparing the results of the neutral salt spray test performed on the samples A, B and C.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example 1:
preparing a copper plating solution, wherein the mass concentration of each component is as follows:
copper carbonate 20g/L
HEDP 170g/L
Potassium carbonate 70g/L
160g/L potassium hydroxide
Bismuth nitrate 0.03g/L
0.005g/L of polycationic quaternary ammonium salt.
Preparing a nickel plating solution, wherein the mass concentration of each component is as follows:
nickel sulfate 20g/L
Sodium hypophosphite 18g/L
Citric acid 10g/L
Malic acid 8g/L
16g/L sodium hydroxide
PPS-OH 0.005g/L
Allyl iodide 0.002 g/L.
Polyquaternium-7 was used as the polycationic quaternary ammonium salt in example 1.
The method adopts the prepared copper plating solution and nickel plating solution, selects a neodymium iron boron permanent magnet sample with the mark of 45M and the specification of 6.0 x 3.5 x 0.45mm for plating, and specifically comprises the following steps:
1) after the neodymium iron boron substrate is degreased, ultrasonically cleaning the neodymium iron boron substrate twice by using clean water, then pickling the neodymium iron boron substrate for 3 minutes by using dilute nitric acid with the concentration of 4%, ultrasonically cleaning the neodymium iron boron substrate twice by using the clean water, adding hydrofluoric acid with the concentration of 1% to activate the neodymium iron boron substrate for 30 seconds, and ultrasonically cleaning the neodymium iron boron substrate twice by using the clean water, namely finishing the pretreatment;
2) putting the pretreated neodymium iron boron substrate into a copper plating solution (the temperature of the copper plating solution is 50 ℃, and the pH value is 9.5-10.0), and carrying out impact electroplating under the action of current to obtain a cyanide-free alkali copper plating layer on the surface of the neodymium iron boron substrate; wherein the current density adopted during electroplating is 0.3ASD, and the electroplating time is 90 min;
3) after the cyanide-free alkali copper plating layer is electroplated, the neodymium iron boron substrate is placed into a nickel plating solution (the temperature of the nickel plating solution is 80 ℃, and the pH value is 4.6-4.8) to carry out chemical nickel plating for 60min, and the neodymium iron boron material after chemical nickel plating is obtained and marked as a sample A.
By performing metallographic test on the sample a, the test result is shown in fig. 1, and it can be seen that: the thickness of the cyanide-free alkali copper plating layer plated on the surface of the neodymium iron boron substrate is 2.87-3.15 mu m, the thickness of the chemical nickel plating layer plated on the surface of the neodymium iron boron substrate is 1.72-2.01 mu m, and the total thickness of the surface plating layer of the neodymium iron boron substrate is about 4.6-5 mu m.
The resulting sample a was then subjected to a neutral salt spray test under the following conditions: the results are shown in Table 1, wherein the temperature is 40 ℃ and the concentration is 5% salt solution, the spraying speed is 2ml/h, and the pH value is 6.8-7.2.
Example 2:
preparing a copper plating solution, wherein the mass concentration of each component is as follows:
27 g/L copper carbonate
HEDP 178g/L
Potassium carbonate 80g/L
160g/L potassium hydroxide
Bismuth nitrate 0.04g/L
0.0035g/L of polycation quaternary ammonium salt.
Preparing a nickel plating solution, wherein the mass concentration of each component is as follows:
nickel sulfate 25g/L
Sodium hypophosphite 20g/L
Citric acid 12g/L
Malic acid 10g/L
18g/L sodium hydroxide
PPS-OH 0.007g/L
Allyl iodide 0.004 g/L.
Polyquaternium-7 was used as the polycationic quaternary ammonium salt in example 2.
The method adopts the prepared copper plating solution and nickel plating solution, selects a neodymium iron boron permanent magnet sample with the mark of 45M and the specification of 6.0 x 3.5 x 0.45mm for plating, and specifically comprises the following steps:
1) after the neodymium iron boron substrate is degreased, ultrasonically cleaning the neodymium iron boron substrate twice by using clean water, then pickling the neodymium iron boron substrate for 3 minutes by using dilute nitric acid with the concentration of 4%, ultrasonically cleaning the neodymium iron boron substrate twice by using the clean water, adding hydrofluoric acid with the concentration of 1% to activate the neodymium iron boron substrate for 30 seconds, and ultrasonically cleaning the neodymium iron boron substrate twice by using the clean water, namely finishing the pretreatment;
2) putting the pretreated neodymium iron boron substrate into a copper plating solution (the temperature of the copper plating solution is 50 ℃, and the pH value is 9.5-10.0), and carrying out impact electroplating under the action of current to obtain a cyanide-free alkali copper plating layer on the surface of the neodymium iron boron substrate; wherein the current density adopted during electroplating is 0.4ASD, and the electroplating time is 70 min;
3) after the cyanide-free alkali copper plating layer is electroplated, the neodymium iron boron substrate is placed into a nickel plating solution (the temperature of the nickel plating solution is 80 ℃, and the pH value is 4.6-5.0) to carry out chemical nickel plating for 60min, and the neodymium iron boron material after chemical nickel plating is obtained and marked as a sample B.
By performing metallographic test on sample B, the test result is shown in fig. 2, and it can be seen that: the thickness of the cyanide-free alkali copper plating layer plated on the surface of the neodymium iron boron substrate is 3.3-3.7 mu m, the thickness of the chemical nickel plating layer plated on the surface of the neodymium iron boron substrate is 1.72-2.01 mu m, and the total thickness of the surface plating layer of the neodymium iron boron substrate is about 5.3-5.5 mu m.
The resulting sample B was then subjected to a neutral salt spray test under the following conditions: the results are shown in Table 1, wherein the temperature is 40 ℃ and the concentration is 5% salt solution, the spraying speed is 2ml/h, and the pH value is 6.8-7.2.
Comparative example 1:
the neodymium iron boron permanent magnet sample is plated, the process steps are repeated in the embodiment 1, the difference is only that the formula composition of the copper plating solution and the nickel plating solution adopted in the plating process of the comparative example 1 is different from that of the embodiment 1, and the other conditions are the same as that of the embodiment.
Comparative example 1 the formulation of the plating solution used in the plating process consists of:
preparing a copper plating solution, wherein the mass concentration of each component is as follows:
copper carbonate 20g/L
HEDP 170g/L
Potassium carbonate 70g/L
160g/L potassium hydroxide
Bismuth nitrate 0.03g/L
Preparing a nickel plating solution, wherein the mass concentration of each component is as follows:
nickel sulfate 20g/L
Sodium hypophosphite 18g/L
Citric acid 10g/L
Malic acid 8g/L
16g/L sodium hydroxide
Allyl iodide 0.002g/L
Comparative example 1 a neodymium iron boron material with a cyanide-free alkaline copper plating and a chemical nickel plating plated on the surface of a neodymium iron boron substrate is marked as sample C.
Through metallographic test on the sample C, the test result is shown in fig. 3, the thickness of the cyanide-free alkali copper plating layer plated on the surface of the neodymium iron boron substrate is 2.87-3.3 μm, the thickness of the chemical nickel plating layer plated on the surface of the neodymium iron boron substrate is 1.58-1.86 μm, and the total thickness of the surface plating layer of the neodymium iron boron substrate is about 4.4-5.2 μm.
The resulting sample C was then subjected to a neutral salt spray test under the following conditions: the results are shown in Table 1, wherein the temperature is 40 ℃ and the concentration is 5% salt solution, the spraying speed is 2ml/h, and the pH value is 6.8-7.2.
And (3) performing neutral salt spray tests on the sample A, the sample B and the sample C, wherein the test method conditions are as follows: the temperature is 40 deg.C, the concentration is 5% salt solution, the spraying speed is 2ml/h, and the pH value is 6.8-7.2. The number of tests on samples B and C was 11, the number of tests on sample a was 10, and the results of neutral salt spray tests on samples a, B, and C are shown in fig. 4.
TABLE 1
As is clear from Table 1 and FIG. 4, the samples A and B prepared in examples 1-2 still maintained good plating at 48 hours after the neutral salt spray test, while the sample C prepared in comparative example 1 showed 2-piece rusting at 48 hours after the neutral salt spray test, indicating that the samples A and B prepared in examples 1-2 have higher corrosion resistance.
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.
Claims (7)
1. An electroplating method of an ultrathin coating for neodymium iron boron is characterized in that the surface of a neodymium iron boron substrate is coated, and an electroplating cyanide-free alkali copper coating and a chemical nickel coating are respectively coated from inside to outside;
the process for electroplating the cyanide-free alkali copper plating layer adopts a copper plating solution, wherein the chemical components of the copper plating solution comprise copper carbonate, HEDP, potassium carbonate, potassium hydroxide, bismuth nitrate and polycation quaternary ammonium salt; the temperature of the copper plating solution is 40-60 ℃, and the pH value is 9-12.
2. The electroplating method of the ultrathin coating for the neodymium-iron-boron as claimed in claim 1, characterized in that the mass concentrations of the chemical components in the copper plating solution are respectively as follows:
20-30 g/L of copper carbonate
HEDP 170-220g/L
70-90g/L potassium carbonate
160g/L potassium hydroxide
0.03-0.08g/L bismuth nitrate
0.001-0.005g/L of polycationic quaternary ammonium salt.
3. The electroplating method of the ultrathin coating for neodymium iron boron as claimed in claim 2, characterized in that the polycationic quaternary ammonium salt is polyquaternium-7, polyquaternium-10 or polyquaternium-22.
4. The method of claim 1, wherein the electroless nickel plating process comprises using a nickel plating solution, the chemical composition of which comprises nickel sulfate, sodium hypophosphite, citric acid, malic acid, sodium hydroxide, PPS-OH, and allyl iodide; the temperature of the nickel plating solution is 75-90 ℃, and the pH value is 4.6-5.0.
5. An electroplating method of an ultrathin coating for neodymium iron boron according to claim 3, characterized in that the mass concentrations of the chemical components in the nickel plating solution are respectively as follows:
nickel sulfate 20-25g/L
18-23g/L sodium hypophosphite
Citric acid 10-15g/L
Malic acid 8-12g/L
16-24g/L of sodium hydroxide
PPS-OH 0.005-0.01g/L
Allyl iodide 0.002-0.007 g/L.
6. The electroplating method of an ultra-thin plated layer for neodymium-iron-boron according to claim 1, wherein the thickness of the cyanide-free alkali copper plated layer is 2-4 μm, and the thickness of the electroless nickel plated layer is 1-2 μm.
7. The electroplating method of the ultrathin coating for the neodymium-iron-boron according to claim 1 is characterized by comprising the following steps:
1) carrying out oil removal, acid washing and activation treatment on the neodymium iron boron substrate before plating;
2) placing the pretreated neodymium iron boron base material into a copper plating solution, and electroplating under the action of current to obtain a cyanide-free alkali copper plating layer on the surface of the neodymium iron boron base material; wherein the current density adopted during electroplating is 0.1-0.5 ASD, and the electroplating time is 60-120 minutes;
3) after the cyanide-free alkali copper plating layer is electroplated, putting the neodymium iron boron base material into a nickel plating solution for chemical nickel plating to obtain a neodymium iron boron material after chemical nickel plating; wherein the temperature for chemical nickel plating is 75-90 ℃ and the time is 40-80 minutes.
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| CN113699567A (en) * | 2021-08-27 | 2021-11-26 | 杭州象限科技有限公司 | Ultrathin plating electroplating method applied to neodymium iron boron surface treatment |
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Application publication date: 20210309 |