CN114892250B - Quick detection method for long-term electroplating applicability of alkaline copper plating solution on surface of neodymium iron boron - Google Patents
Quick detection method for long-term electroplating applicability of alkaline copper plating solution on surface of neodymium iron boron Download PDFInfo
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- CN114892250B CN114892250B CN202210638747.4A CN202210638747A CN114892250B CN 114892250 B CN114892250 B CN 114892250B CN 202210638747 A CN202210638747 A CN 202210638747A CN 114892250 B CN114892250 B CN 114892250B
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Abstract
The invention provides a method for rapidly detecting the long-term electroplating applicability of an alkaline copper plating solution on the surface of neodymium iron boron, which comprises the following steps: 1) Preparing an alkaline copper plating solution; 2) Measuring a stable open circuit potential value of the copper electrode in the prepared solution; 3) Measuring a stable open circuit potential value of the NdFeB electrode in the prepared solution, and calculating a difference value between the stable open circuit potential value and the open circuit potential of the copper electrode measured in the step 2), so as to perform first applicability judgment; 4) Measuring the self-corrosion current density of the neodymium-iron-boron magnet in the prepared copper plating solution, so as to carry out second applicability judgment; 5) And measuring the time-potential curve of the NdFeB magnet in the prepared solution, so as to carry out third suitability judgment. Compared with the method for observing whether the copper replacement layer exists on the surface of the neodymium iron boron after the plating solution is soaked for a long time, the method is higher in detection accuracy and speed, can be used for indicating the possible problems in a long production period in advance, and greatly reduces the trial-and-error period and cost in production.
Description
Technical Field
The invention relates to a judging method of plating solution applicability, in particular to a rapid detection method of long-term plating applicability of alkaline copper plating solution on the surface of neodymium iron boron.
Background
Neodymium iron boron magnets are functional materials that are widely used in the field of electronic devices. The chemical property is active, the corrosion is easy, and the surface is mostly protected by adopting a nickel plating layer at present. In order to improve the bonding force between the plating layer and the substrate interface and reduce the damage of hydrogen evolution reaction to the magnet during nickel plating, a copper bottom layer is generally required to be plated on the surface. However, copper has a higher potential than neodymium iron boron, and copper ions tend to replace neodymium and iron ions, so that a replacement copper layer is easily formed on the surface, and the interfacial bonding force of the plating layer is reduced. In addition, the dissolved neodymium iron and other elements gradually accumulate, and when the amount exceeds a certain amount, the liquid plating performance is seriously deteriorated, so that the production requirements cannot be continuously met.
The long-term electroplating of the unacceptable copper plating solution can present the following problems:
(1) Copper ions tend to replace neodymium and iron ions, so that a replaced copper layer is easily formed on the surface, and the interface binding force of the plating layer is reduced.
(2) The dissolved neodymium iron and other elements gradually accumulate, and when the amount exceeds a certain amount, the plating solution performance is seriously deteriorated.
It is believed that the use of suitable, high concentrations of complex and higher pH values can alleviate the problem of copper substitution. However, the plating solution containing the components can meet the long-term electroplating production requirement, and no definite quantitative standard exists at present. Conventionally, a plating solution soaking method is generally adopted, and the time for obviously replacing the copper layer on the surface is observed. However, for longer production cycles, even small amounts of copper substitution gradually accumulate to impurity levels outside the process tolerance range, which cannot be demonstrated in shorter soak experiments. Therefore, the applicability of the plating solution in long-term use needs to be linked with certain specific measurable physical and chemical parameters thereof so as to achieve the aim of rapid judgment.
In view of this, the present invention has been made.
Disclosure of Invention
Aiming at the problem that the plating solution lacks a standard for definite quantification in the prior art, the invention aims to provide an electrochemical detection method, which aims to rapidly and accurately judge the suitability of alkaline copper plating solution for long-term electroplating on the surface of neodymium iron boron so as to select a proper alkaline copper plating solution.
In order to achieve the above purpose, the invention provides a rapid detection method for the suitability of alkaline copper plating solution for long-term electroplating on the surface of neodymium iron boron, which comprises the following steps:
(1) Preparing an alkaline copper plating solution;
(2) Measuring a stable open circuit potential value of the copper electrode in the prepared solution;
more preferably, in the step (1), the solution contains a main complexing agent and an auxiliary complexing agent, the main complexing agent is HEDP, and the auxiliary complexing agent is sodium gluconate.
More preferably, in the step (2), a three-electrode system of an electrochemical workstation is used for testing, a platinum sheet is used as a counter electrode, and red copper with purity more than or equal to 99.95wt.% is used as a copper electrode.
More preferably, in the step (2), the criterion for achieving the stability of the open circuit potential is: the potential fluctuation value is less than or equal to 5mV in 60 seconds, and the stable potential value is the average value of the upper limit and the lower limit of the potential fluctuation.
(3) Measuring a stable open-circuit potential value of the NdFeB electrode in the solution prepared in the step (1), calculating a difference value between the stable open-circuit potential value and the open-circuit potential of the copper electrode measured in the step (2), judging the applicability for the first time, and if the applicability meets the requirement, performing the step (4);
more preferably, in the step (3), the test is performed by using an electrochemical workstation three-electrode system, a platinum sheet is used as a counter electrode, and the standard that the open circuit potential reaches stability is: the potential fluctuation value is less than or equal to 10mV in 60 seconds, and the stable potential value is the average value of the upper limit and the lower limit of the potential fluctuation.
The basis for the first applicability judgment is as follows: if the absolute value of the stable open circuit potential difference value of the neodymium iron boron and the red copper plate is more than or equal to 200mV, the test is terminated, and the alkaline copper plating solution in the step (1) is judged to be unsuitable for long-term electroplating of the neodymium iron boron surface. And (4) if the absolute value of the stable open circuit potential difference value of the NdFeB and the red copper plate is less than 200 mV.
(4) Measuring the self-corrosion current density of the neodymium-iron-boron electrode in the copper plating solution prepared in the step (1), judging the applicability of the copper plating solution for the second time, and if the applicability meets the requirement, performing the step (5);
more preferably, in the step (4), the test is performed by using an electrochemical workstation three-electrode system, a platinum sheet is used as a counter electrode, and the self-corrosion current density is measured and calculated by adopting a tafel curve strong polarization area linear extrapolation method. When a tafel plot measurement is performed, the potential is swept from an open circuit potential of plus 200mV to an open circuit potential of minus 200 mV.
The basis for carrying out the second applicability judgment is as follows: if the measured self-corrosion current density is more than or equal to 1 multiplied by 10 -5 A/cm 2 And (3) terminating the test, and judging that the alkaline copper plating solution in the step (1) is not suitable for long-term electroplating of the surface of the neodymium iron boron. If it is calculatedSelf-etching current density<1×10 -5 A/cm 2 Step (5) is performed.
(5) Determining a time-open circuit potential curve of the neodymium-iron-boron electrode in the solution prepared in the step (1), judging the applicability of the third time according to the time-open circuit potential curve, and judging that the alkaline copper plating solution prepared in the step (1) can be used for long-term electroplating of the neodymium-iron-boron surface if the applicability is satisfactory;
more preferably, in the step (5), the test is performed by using an electrochemical workstation three-electrode system, and the measurement time of the open-circuit potential-time curve is more than or equal to 20 minutes by using a platinum sheet as a counter electrode.
The basis for the third suitability determination is as follows: if the average descending speed of the potential in the open circuit potential-open circuit time curve is less than or equal to 20mV/20min, judging that the alkaline copper plating solution in the step (1) is suitable for long-term electroplating of the surface of the neodymium iron boron; if the average dropping speed of the potential in the open circuit potential-open circuit time curve is more than 20mV/20min, the alkaline copper plating solution in the step (1) is judged to be not suitable for long-term electroplating of the surface of the neodymium iron boron.
Technical effects
Compared with the prior art, the invention has the beneficial effects that: the suitability of the alkaline copper plating solution for long-term electroplating on the surface of the neodymium iron boron material can be rapidly and accurately judged through electrochemical measurement. Compared with a general soaking method, the method has the advantages that the testing time is greatly shortened, and more importantly, the tendency and the speed of copper substitution and corrosion dissolution of neodymium iron boron in the plating solution can be accurately reflected. Sometimes weaker displacement and corrosion can accumulate to a degree outside the process tolerances during long-term production operations, which is not readily apparent by soaking.
Drawings
FIG. 1 is a graph showing the open circuit potential of the copper plate and NdFeB obtained in example 1 of the present invention in an HEDP copper plating solution within 100 seconds.
FIG. 2 is a graph showing the open circuit potential of the copper plate and NdFeB obtained in example 2 of the present invention in an HEDP copper plating solution within 100 seconds.
FIG. 3 is a Tafil curve of NdFeB in an HEDP alkaline copper plating solution tested in example 2 of the present invention.
FIG. 4 is a graph showing the time-open circuit potential of NdFeB in an HEDP alkaline copper plating solution tested in example 2 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below. It will be apparent that the described embodiments are only some, but not all, embodiments of the invention. All other embodiments, based on the examples herein, which are within the scope of the invention as defined by the claims, will be within the scope of the invention as defined by the claims.
In order to achieve the above purpose, the embodiment of the invention provides a rapid detection method for the long-term electroplating applicability of an alkaline copper plating solution on the surface of neodymium iron boron, which specifically comprises the following steps:
(1) Preparing an alkaline copper plating solution, wherein the solution is prepared according to the upper limit of the concentration of main salt and the lower limit of the pH value of the formula;
(2) Measuring a stable open circuit potential value of the copper electrode in the prepared solution;
the method provided by the invention is suitable for various alkaline copper plating solutions. In one embodiment of the present invention, in the step (1), the primary salt includes a primary complexing agent and a secondary complexing agent. The primary complexing agent has a variety of options depending on the system, for example HEDP (collectively referred to as hydroxyethylidene diphosphonic acid or hydroxyethylidene diphosphonic acid) is one of them, and the secondary complexing agent such as sodium gluconate, and the like.
In one embodiment of the present invention, in the step (2), the test is performed using an electrochemical workstation three-electrode system, a platinum sheet is used as a counter electrode, and copper electrodes are made of red copper with a purity of 99.95wt.% or more.
In one embodiment of the present invention, in the step (2), the criterion that the open circuit potential is stabilized is: the potential fluctuation value is less than or equal to 5mV in 60 seconds, and the stable potential value is the average value of the upper limit and the lower limit of the potential fluctuation. Since the open circuit potential generally fluctuates with time, the electrode may react with the solution just after entering the solution, the surface state changes, and the open circuit potential fluctuates relatively greatly. After the waiting reaction is stable, the open circuit potential is generally stable and the fluctuation is small. Therefore, the artificial limitation of the fluctuation value to be less than or equal to 5mV shows that the potential fluctuation is small at the moment, so that a stable state is achieved, and the data reading is convenient.
(3) Measuring a stable open circuit potential value of the NdFeB electrode in the solution prepared in the step (1), calculating a difference value between the stable open circuit potential value and the open circuit potential of the copper electrode measured in the step (2), and judging the applicability for the first time, namely judging whether a copper substitution reaction occurs or not, and if the copper substitution reaction meets the requirement, carrying out the step (4);
in one embodiment of the present invention, in the step (3), the test is performed using an electrochemical workstation three-electrode system, and the platinum sheet is used as the counter electrode, and the standard that the open circuit potential is stable is: the potential fluctuation value is less than or equal to 10mV in 60 seconds, and the stable potential value is the average value of the upper limit and the lower limit of the potential fluctuation.
The basis for the first applicability judgment is as follows: if the absolute value of the stable open circuit potential difference value of the neodymium iron boron and the red copper plate is more than or equal to 200mV, the test is terminated, and the alkaline copper plating solution in the step (1) is judged to be unsuitable for long-term electroplating of the neodymium iron boron surface. If the absolute value of the stable open circuit potential difference value of the NdFeB and the red copper plate is less than 200mV, continuing to carry out the subsequent steps.
The absolute value of the stable open circuit potential difference value of the NdFeB and the red copper plate is limited to be more than or equal to 200mV, and the stable open circuit potential difference value is also artificially established. The open circuit potential of the red copper plate reflects the oxidation-reduction potential of copper ions in the solution, and the larger the difference between the oxidation-reduction potential and the open circuit potential of neodymium iron boron is, the stronger the tendency of the copper ions in the solution to replace the neodymium iron boron is. When the trend of replacing the neodymium iron boron with copper is strong, the bonding force of a plating layer interface is weak, and the replaced neodymium iron boron enters the plating solution to cause pollution of the plating solution, so that the performance of the plating solution is reduced.
(4) Measuring the self-corrosion current density of the NdFeB electrode in the copper plating solution prepared in the step (1), judging the applicability for the second time, namely judging the corrosion speed in a short time, and if the corrosion speed meets the requirement, performing the step (5);
in one embodiment of the present invention, in the step (4), the test is performed using an electrochemical workstation three-electrode system, and the self-corrosion current density is measured by using a tafel curve strong polarization area linear extrapolation method with a platinum sheet as a counter electrode. When a tafel plot measurement is performed, the potential is swept from an open circuit potential of plus 200mV to an open circuit potential of minus 200 mV.
The basis for carrying out the second applicability judgment is as follows: if the measured self-corrosion current density is more than or equal to 1 multiplied by 10 -5 A/cm 2 And (3) terminating the test, and judging that the alkaline copper plating solution in the step (1) is not suitable for long-term electroplating of the surface of the neodymium iron boron. If the self-corrosion current density is calculated<1×10 -5 A/cm 2 The subsequent steps are continued. Since the self-corrosion current density of NdFeB reflects the corrosion speed of NdFeB in the plating solution, the maximum allowable self-corrosion speed is artificially established aiming at the characteristic.
(5) Determining a time-open circuit potential curve of the neodymium-iron-boron electrode in the solution prepared in the step (1), judging the applicability for the third time, namely judging the long-time corrosion speed, and judging that the alkaline copper plating solution prepared in the step (1) can be used for long-time electroplating of the neodymium-iron-boron surface if the corrosion speed meets the requirement;
in one embodiment of the present invention, in the step (5), the test is performed using an electrochemical workstation three-electrode system, and the measurement time of the open-circuit potential-time curve is equal to or longer than 20 minutes with a platinum sheet as a counter electrode.
The basis for the third suitability determination is as follows: if the average descending speed of the potential in the open circuit potential-open circuit time curve is less than or equal to 20mV/20min, the alkaline copper plating solution in the step (1) is judged to be suitable for long-term electroplating of the surface of the neodymium iron boron. If the average dropping speed of the potential in the open circuit potential-open circuit time curve is more than 20mV/20min, the alkaline copper plating solution in the step (1) is judged to be not suitable for long-term electroplating of the surface of the neodymium iron boron. Since alkaline copper plating solution can cause corrosion to a certain extent on the neodymium iron boron material, the corrosion can lead to gradual decrease of open circuit potential of the neodymium iron boron. The stronger the corrosion, the more pronounced the potential drop. There is artificially defined a maximum allowable descent speed.
Example 1
The invention provides a method for rapidly detecting the long-term electroplating applicability of an alkaline copper plating solution on the surface of neodymium iron boron, which comprises the following specific process steps:
1. preparing plating solution according to the upper limit of the concentration of main salt in a conventional HEDP copper plating process formula, wherein the specific components are 60g/L of copper sulfate pentahydrate, 215g/L of HEDP and 12g/L of auxiliary complexing agent (sodium gluconate) by K 2 CO 3 And KOH mixed solution to adjust the pH value to 8.5;
2. the open circuit potential of the red copper plate with the purity of 99.99% is tested by using an electrochemical workstation three-electrode system, a platinum sheet is a counter electrode, a reference electrode is a saturated calomel electrode, the whole potential is found to be stable after the test duration is 100s, the fluctuation value is smaller than 5mV/60s, and the test is stopped, so that the result is shown in figure 1. The stable open circuit potential of the copper plate is about-0.37V calculated by the figure 1;
3. the open-circuit potential of neodymium iron boron is tested by using an electrochemical workstation three-electrode system, a platinum sheet is a counter electrode, a reference electrode is a saturated calomel electrode, the whole potential is found to be stable after the test duration is 100s, the fluctuation value is smaller than 10mV/60s, and the test is stopped. As can be seen from FIG. 1, the potential of the NdFeB initially drops significantly over time, and then gradually stabilizes, and the fluctuation in the post 60s is less than 5mV, so that the stable open circuit potential of the NdFeB is calculated to be about-0.62V according to the curve of the post 60s, the difference between the open circuit potential and the value of the NdFeB is 250mV, exceeds 200mV, the test is terminated, and the plating solution is judged to be unsuitable for long-term electroplating of the NdFeB surface.
Example 2
The invention provides a method for rapidly detecting the long-term electroplating applicability of an alkaline copper plating solution on the surface of neodymium iron boron, which comprises the following specific process steps:
1. preparing plating solution according to the upper limit of the concentration of main salt in a HEDP copper plating process formula, wherein the specific components are 30g/L of copper acetate, 90g/L of HEDP and 30g/L of auxiliary complexing agent (sodium gluconate) by K 2 CO 3 And KOH mixed solution to adjust the pH value to 8.8;
2. the open circuit potential of the red copper plate with the purity of 99.99% is tested by using an electrochemical workstation three-electrode system, a platinum sheet is a counter electrode, a reference electrode is a saturated calomel electrode, the whole potential is found to be stable after the test duration is 65 seconds, the fluctuation value is smaller than 5mV/60 seconds, and the test is stopped, so that the result is shown in figure 2. The average stable open circuit potential value of the copper plate is about-0.53V calculated by the graph of FIG. 2;
3. the open-circuit potential of the neodymium iron boron is tested by using an electrochemical workstation three-electrode system, a platinum sheet is a counter electrode, a reference electrode is a saturated calomel electrode, the whole potential is found to be stable after the test duration is 65 seconds, the fluctuation value is smaller than 10mV/60 seconds, and the test is stopped. The stable open circuit potential of NdFeB was calculated from FIG. 2 to be about-0.69V, which is 160mV different from the value of the copper plate, less than 200mV, and it was determined that the subsequent steps could be continued.
4. The open-circuit potential of the neodymium iron boron is tested by using an electrochemical workstation three-electrode system, a platinum sheet is a counter electrode, a reference electrode is a saturated calomel electrode, a Tafil curve of the neodymium iron boron in alkaline copper plating solution is measured, and the potential is scanned from the positive direction to the negative direction during the test, and the result is shown in figure 3. As measured by linear extrapolation of the strongly polarized region in FIG. 3, as shown by dotted lines in FIG. 3, the tangential lines at two ends of the polarization curve are extended and intersected, and the current density at the intersection point is NdFeB self-corrosion current density less than 1×10 -5 A/cm 2 Judging to continue to follow the following steps;
5. the open-circuit potential of the neodymium iron boron is tested by using an electrochemical workstation three-electrode system, a platinum sheet is a counter electrode, a reference electrode is a saturated calomel electrode, the time-open-circuit potential curve of the neodymium iron boron in alkaline copper plating solution is measured, the test time is 30min, and the result is shown in figure 4. The open circuit potential initially drops around-0.655V gradually over time, has dropped to about-0.67V at 30min, drops by about 15mV at 30min, and the average drop rate is less than 20mV/20min, and the alkaline copper plating solution is determined to be suitable for long-term electroplating of neodymium iron boron surfaces.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any person skilled in the art will readily recognize that variations or substitutions are within the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (3)
1. The method for rapidly detecting the long-term electroplating applicability of the alkaline copper plating solution on the surface of the neodymium iron boron is characterized by comprising the following steps of:
(1) Preparing an alkaline copper plating solution;
(2) Measuring the stable open circuit potential value of the copper electrode in the solution prepared in the step (1);
(3) Measuring a stable open-circuit potential value of the NdFeB electrode in the solution prepared in the step (1), calculating a difference value between the stable open-circuit potential value and the open-circuit potential of the copper electrode measured in the step (2), judging the applicability for the first time, and if the applicability meets the requirement, performing the step (4);
(4) Measuring the self-corrosion current density of the neodymium-iron-boron electrode in the copper plating solution prepared in the step (1), judging the applicability of the copper plating solution for the second time, and if the applicability meets the requirement, performing the step (5);
(5) Determining a time-open circuit potential curve of the neodymium-iron-boron electrode in the solution prepared in the step (1), judging the applicability of the third time according to the time-open circuit potential curve, and judging that the alkaline copper plating solution prepared in the step (1) can be used for long-term electroplating of the neodymium-iron-boron surface if the applicability is satisfactory;
in the step (2), the criterion for the open circuit potential to reach stability is: the potential fluctuation value is less than or equal to 5mV within 60 seconds, and the stable potential value is the average value of the upper limit and the lower limit of the potential fluctuation;
in the step (3), the test is performed by using an electrochemical workstation three-electrode system, a platinum sheet is used as a counter electrode, and the standard that the open circuit potential reaches stability is as follows: the potential fluctuation value is less than or equal to 10mV within 60 seconds, and the stable potential value is the average value of the upper limit and the lower limit of the potential fluctuation;
in the step (3), the basis for performing the first applicability judgment is as follows: if the absolute value of the stable open-circuit potential difference value of the neodymium iron boron and the red copper plate is more than or equal to 200 and mV, terminating the test, and judging that the alkaline copper plating solution in the step (1) is not suitable for long-term electroplating of the neodymium iron boron surface; if the absolute value of the stable open-circuit potential difference value of the NdFeB and the red copper plate is less than 200mV, performing the step (4);
in the step (4), testing is carried out by using a three-electrode system of an electrochemical workstation, a platinum sheet is used as a counter electrode, and self-corrosion current density is measured and calculated by adopting a Tafil curve strong polarization area linear extrapolation method; when the tafel plot measurement is carried out, the potential starts to scan from the open circuit potential of plus 200mV to the open circuit potential of minus 200 mV;
in the step (4), the basis for performing the second applicability judgment is as follows: if the measured self-corrosion current density is more than or equal to 1 multiplied by 10 -5 A/cm 2 Terminating the test, and judging that the alkaline copper plating solution in the step (1) is not suitable for long-term electroplating of the surface of the neodymium iron boron; if the self-corrosion current density is calculated<1×10 -5 A/cm 2 Step (5) is carried out;
in the step (5), a three-electrode system of an electrochemical workstation is used for testing, a platinum sheet is used as a counter electrode, and the measuring time of an open-circuit potential-time curve is more than or equal to 20 minutes;
in the step (5), the basis for performing the third applicability judgment is as follows: if the average descending speed of the potential in the open circuit potential-open circuit time curve is less than or equal to 20mV/20min, judging that the alkaline copper plating solution in the step (1) is suitable for long-term electroplating of the surface of the neodymium iron boron; if the average dropping speed of the potential in the open circuit potential-open circuit time curve is more than 20mV/20min, the alkaline copper plating solution in the step (1) is judged to be not suitable for long-term electroplating of the NdFeB surface.
2. The method according to claim 1, wherein in the step (1), the solution contains a main complexing agent and an auxiliary complexing agent, the main complexing agent is HEDP, and the auxiliary complexing agent is sodium gluconate.
3. The method according to claim 1, wherein in the step (2), a three-electrode system of an electrochemical workstation is used for testing, a platinum sheet is used as a counter electrode, and copper with purity not less than 99.95 and wt% is used as a copper electrode.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2016114391A (en) * | 2014-12-11 | 2016-06-23 | 凸版印刷株式会社 | Electric copper plating solution analysis device and electric copper plating solution analysis method |
| CN109161941A (en) * | 2018-08-09 | 2019-01-08 | 浙江工业大学 | A kind of Sintered NdFeB magnet copper composite graphite alkene coating bottoming is to improve corrosion proof method and product |
| CN111334828A (en) * | 2020-04-03 | 2020-06-26 | 包头汇众磁谷稀土科技有限公司 | Surface treatment method for neodymium iron boron permanent magnet material and product |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2016114391A (en) * | 2014-12-11 | 2016-06-23 | 凸版印刷株式会社 | Electric copper plating solution analysis device and electric copper plating solution analysis method |
| CN109161941A (en) * | 2018-08-09 | 2019-01-08 | 浙江工业大学 | A kind of Sintered NdFeB magnet copper composite graphite alkene coating bottoming is to improve corrosion proof method and product |
| CN111334828A (en) * | 2020-04-03 | 2020-06-26 | 包头汇众磁谷稀土科技有限公司 | Surface treatment method for neodymium iron boron permanent magnet material and product |
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