CN104120469B - Neodymium iron boron magnetic body method for electroplating nickel - Google Patents
Neodymium iron boron magnetic body method for electroplating nickel Download PDFInfo
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- CN104120469B CN104120469B CN201410263544.7A CN201410263544A CN104120469B CN 104120469 B CN104120469 B CN 104120469B CN 201410263544 A CN201410263544 A CN 201410263544A CN 104120469 B CN104120469 B CN 104120469B
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Abstract
The invention discloses a kind of neodymium iron boron magnetic body method for electroplating nickel, specifically comprise neodymium iron boron magnetic body is carried out to pre-treating technology, nickel preplating, washing process, plate half light nickel technique, washing process, bright nickel plating technique and washing process, in nickel preplating, adopt by nickelous sulfate, boric acid, succinate sodium salt, the first electronickelling solution of carboxyethyl sodium sulfonate and water composition, in plating half light nickel processing procedure, adopt by nickelous sulfate, diammonium hydrogen citrate, boric acid, the second electronickelling solution of ammoniacal liquor and water composition, in the first electronickelling solution, do not contain chlorion, in the first electronickelling solution, contain succinate sodium salt and carboxyethyl sodium sulfonate, in the second electronickelling solution, contain appropriate diammonium hydrogen citrate, advantage is to reduce the impact of the magnetic property of electroplating process on neodymium iron boron magnetic body, ensures that neodymium iron boron magnetic body has good magnetic property, and while electroplating for the less product of end angle, its being uniformly distributed property of thickness of coating is also better.
Description
Technical field
The present invention relates to a kind of electro-plating method, especially relate to a kind of neodymium iron boron magnetic body method for electroplating nickel.
Background technology
Galvanizer's artistic skill effectively plays decorative and protective effect to magnet, has been widely used at present neodymium-iron-boron surfaceProtective treatment. Electroplating technology kind is a lot, such as techniques such as electronickelling, electro-coppering and electrotinnings. Wherein electronickelling techniqueThe electroless nickel layer crystallization forming in neodymium-iron-boron surface is tiny, and property stable in the air is high, is that use is more at presentA kind of electroplating technology. The electronickelling technique of existing neodymium iron boron magnetic body mainly comprises nickel preplating, half light nickel and bright nickel, pre-The electroplate liquid being formed by nickelous sulfate, nickel chloride and boric acid adopting in nickel plating technology, in half light nickel technique, adopt be byThe electroplate liquid of nickelous sulfate, nickel chloride, boric acid and half brightener composition, what in bright nickel technique, adopt is by nickelous sulfate, chlorineChange the electroplate liquid of nickel, boric acid and brightener composition. But there is following problem in the electronickelling technique of existing neodymium iron boron magnetic body:One, in one side nickel preplating, electrode pair neodymium iron boron magnetic body magnetic property causes harmful effect, on the other hand due to nickel preplatingThere is chlorion in the electroplate liquid using in technique, and neodymium iron boron magnetic body directly contacts with chlorion in nickel preplating, neodymiumIron boron magnet matrix, by chloride ion corrosion, causes the magnetic property decline of the neodymium iron boron magnetic body after having electroplated more, magnetic thusPoor-performing; Two, for the less product of end angle (thering is the product of tip portion), due to point discharge effectShould, in electroplating process, more electrons, in the most advanced and sophisticated gathering of neodymium iron boron magnetic body, causes a large amount of nickel ion discharge depositings, thusCause being uniformly distributed property of thickness of coating poor.
Summary of the invention
Technical problem to be solved by this invention is to provide and a kind ofly can reduces the magnetic property of electroplating process to neodymium iron boron magnetic bodyImpact, ensure that neodymium iron boron magnetic body has good magnetic property, and while electroplating for the less product of end angle,Its being uniformly distributed property of thickness of coating is good neodymium iron boron magnetic body method for electroplating nickel also.
The present invention solves the problems of the technologies described above adopted technical scheme: a kind of neodymium iron boron magnetic body method for electroplating nickel, comprisesFollowing steps:
1. neodymium iron boron magnetic body is carried out to pre-treatment;
2. nickel preplating: the neodymium iron boron magnetic body after pre-treatment is put into the first electronickelling solution and carry out nickel preplating processing, timeBe 2500～5500 seconds, wherein the first electronickelling solution is by nickelous sulfate, boric acid, succinate sodium salt, carboxyethyl sulfonic acidSodium and water composition, the mass body volume concentrations of nickelous sulfate is 220～380 grams per liters, the mass body volume concentrations of boric acid is 30～60Grams per liter, the mass body volume concentrations of succinate sodium salt is 5～20 mg/litre, the mass body volume concentrations of carboxyethyl sodium sulfonateBe 5～20 mg/litre, in nickel preplating processing procedure, current density is 0.1～0.6 ampere/square decimeter, and first electroplatesThe temperature of nickel solution is 40～65 degrees Celsius, and pH value is 3.5～4.8;
3. the neodymium iron boron magnetic body that adopts deionized water to process nickel preplating repeatedly cleans;
4. plate half light nickel: the neodymium iron boron magnetic body after cleaning is put into the second electronickelling solution and plate half light nickel processing, timeBetween be 3500～6500 seconds, the second electronickelling solution is made up of nickelous sulfate, diammonium hydrogen citrate, boric acid, ammoniacal liquor and water,The mass body volume concentrations of nickelous sulfate is 100～210 grams per liters, and the mass body volume concentrations of diammonium hydrogen citrate is 65～145 grams/ liter, the mass body volume concentrations of boric acid is 10～40 grams per liters, the volumetric concentration of ammoniacal liquor is 20～60 milliliters/liter, plating halfIn light nickel processing procedure, current density is 0.2～0.7 ampere/square decimeter, and the temperature of the second electronickelling solution is 40～65Degree Celsius, pH value is 5.5～7.5;
5. adopt deionized water repeatedly to clean the neodymium iron boron magnetic body that plates half light nickel and processed, in cleaning process, arrangeHave Ultrasonic Cleaning, ultrasonic power is 2000W, and frequency is 20～60KHz;
6. bright nickel plating: the neodymium iron boron magnetic body after cleaning is put into the 3rd electronickelling solution and carry out bright nickel plating processing, timeBetween be 2500～5500 seconds, the 3rd electronickelling solution is made up of nickelous sulfate, nickel chloride, boric acid, saccharin sodium and water, sulphurThe mass body volume concentrations of acid nickel is 220～380 grams per liters, and the mass body volume concentrations of nickel chloride is 20～60 grams per liters, boronThe mass body volume concentrations of acid is 30～60 grams per liters, and the mass body volume concentrations of saccharin sodium is 5～20 mg/litre, and light-plated is brightIn nickel processing procedure, current density is 0.1～0.6 ampere/square decimeter, and the temperature of the 3rd electronickelling solution is 40～65Degree Celsius, pH value is 3.5～4.8;
7. the neodymium iron boron magnetic body that adopts deionized water to process bright nickel plating repeatedly cleans, and in cleaning process, is provided withUltrasonic Cleaning, ultrasonic power is 2000W, frequency is 40～138KHz.
Described pre-treating technology comprises the following steps:
1.-1 pickling: adopt dilute nitric acid solution, as pickle, neodymium iron boron magnetic body is carried out to pickling;
1.-2 washings: the neodymium iron boron magnetic body after adopting deionized water to pickling repeatedly cleans, and is provided with in cleaning processUltrasonic Cleaning, ultrasonic power is 2000W, frequency is 20～60KHz;
1. the neodymium iron boron magnetic body after washing is put into electrolytic cell by-3 carries out electrolytic treatments, and the electrolytic treatments time is 200～450Second, electrolyte is made up of NaOH, sodium carbonate and water, and the mass body volume concentrations of NaOH is 20～60 grams per liters,The mass body volume concentrations of sodium carbonate is 10～40 grams per liters, in electrolytic treatments process current density be 0.2～0.7 ampere/flatSide's decimetre, electrolyte temperature is 30～60 degrees Celsius;
1.-4 washings: the neodymium iron boron magnetic body after adopting deionized water to electrolysis repeatedly cleans, and is provided with in cleaning processUltrasonic Cleaning, ultrasonic power is 2000W, frequency is 20～60KHz.
Compared with prior art, the invention has the advantages that first in nickel preplating processing procedure, adopt by nickelous sulfate, boric acid,The first electronickelling solution of succinate sodium salt, carboxyethyl sodium sulfonate and water composition, does not contain chlorine in the first electronickelling solutionIon, has eliminated chlorion corrodes the neodymium iron boron magnetic body magnetic property causing decline to neodymium iron boron magnetic body, and the first electronickelling is moltenIn liquid, each component is configured according to the mass body volume concentrations adapting to, and ensures to form fine and close preplating in neodymium-iron-boron surfaceNickel dam, in addition, succinate sodium salt and carboxyethyl sodium sulfonate in the first electronickelling solution, due to succinate sodium salt and carboxylicThe existence of ethylsulfonic acid sodium, has reduced the impact of electrode side reaction on neodymium iron boron magnetic body magnetic property in electroplating process, ensures neodymiumIron boron magnet has good magnetic property, then in plating half light nickel processing procedure, adopt by nickelous sulfate, diammonium hydrogen citrate,The second electronickelling solution of boric acid, ammoniacal liquor and water composition, contains appropriate diammonium hydrogen citrate in the second electronickelling solution,Increase the polarizability of cathodic process in electroplating process, reduced the product electrodeposited coating thickness that electroplating process is less to end angleImpact, improve being uniformly distributed property of neodymium iron boron magnetic body thickness of coating, make being uniformly distributed property of neodymium iron boron magnetic body thickness of coating better;
In the time adopting following pre-treating technology to carry out pre-treatment to neodymium iron boron magnetic body: pickling: adopt dilute nitric acid solution as acidWashing lotion is carried out pickling to neodymium iron boron magnetic body; Washing: the neodymium iron boron magnetic body after adopting deionized water to pickling carries out repeatedly clearWash, be provided with Ultrasonic Cleaning in cleaning process, ultrasonic power is 2000W, and frequency is 20～60KHz; To washAfter neodymium iron boron magnetic body put into electrolytic cell and carry out electrolytic treatments, the electrolytic treatments time is 200～450 seconds, electrolyte byNaOH, sodium carbonate and water composition, the mass body volume concentrations of NaOH is 20～60 grams per liters, the matter of sodium carbonateAmount volumetric concentration is 10～40 grams per liters, and in electrolytic treatments process, current density is 0.2～0.7 ampere/square decimeter, electricitySeparating liquid temp is 30～60 degrees Celsius; Washing: the neodymium iron boron magnetic body after adopting deionized water to electrolysis repeatedly cleans,In cleaning process, be provided with Ultrasonic Cleaning, ultrasonic power is 2000W, and frequency is 20～60KHz; First in picklingMiddle employing dilute nitric acid solution is as pickle, and rare nitric acid and neodymium-iron-boron precursor reactant can not cause damage to neodymium-iron-boron body structureEvil, reduces the impact of pickling on magnetic property, then adopts the technique of washing, electrolysis and washing again to enter neodymium iron boron magnetic bodyRow is processed, and can remove greasy dirt and oxide on surface etc. that neodymium iron boron magnetic body produces in preceding working procedure, ensures neodymium-iron-boronSurface, entering before groove in activated state, has good cleannes and magnetic property.
Brief description of the drawings
Fig. 1 is the structural representation of neodymium iron boron magnetic body product in embodiment.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail.
Embodiment mono-: a kind of neodymium iron boron magnetic body method for electroplating nickel, comprises the following steps:
1. neodymium iron boron magnetic body is carried out to pre-treatment;
2. nickel preplating: the neodymium iron boron magnetic body after pre-treatment is put into the first electronickelling solution and carry out nickel preplating processing, timeBe 3500 seconds, wherein the first electronickelling solution is by nickelous sulfate, boric acid, succinate sodium salt, carboxyethyl sodium sulfonate and waterComposition, the mass body volume concentrations of nickelous sulfate is 250 grams per liters, the mass body volume concentrations of boric acid is 40 grams per liters, butanedioic acidThe mass body volume concentrations of ester sodium salt is 5 mg/litre, and the mass body volume concentrations of carboxyethyl sodium sulfonate is 5 mg/litre, preplatingIn nickel processing procedure, current density is 0.2 ampere/square decimeter, and the temperature of the first electronickelling solution is 45 degrees Celsius, pHValue is 4.1;
3. the neodymium iron boron magnetic body that adopts deionized water to process nickel preplating repeatedly cleans;
4. plate half light nickel: the neodymium iron boron magnetic body after cleaning is put into the second electronickelling solution and plate half light nickel processing, timeBetween be 4500 seconds, the second electronickelling solution is made up of nickelous sulfate, diammonium hydrogen citrate, boric acid, ammoniacal liquor and water, sulfuric acidThe mass body volume concentrations of nickel is 150 grams per liters, and the mass body volume concentrations of diammonium hydrogen citrate is 80 grams per liters, the matter of boric acidAmount volumetric concentration is 10 grams per liters, and the volumetric concentration of ammoniacal liquor is 20 milliliters/liter, current density in plating half light nickel processing procedureBe 0.2 ampere/square decimeter, the temperature of the second electronickelling solution is 45 degrees Celsius, and pH value is 6.5;
5. adopt deionized water repeatedly to clean the neodymium iron boron magnetic body that plates half light nickel and processed, in cleaning process, arrangeHave Ultrasonic Cleaning, ultrasonic power is 2000W, and frequency is 20KHz;
6. bright nickel plating: the neodymium iron boron magnetic body after cleaning is put into the 3rd electronickelling solution and carry out bright nickel plating processing, timeBetween be 3500 seconds, the 3rd electronickelling solution is made up of nickelous sulfate, nickel chloride, boric acid, saccharin sodium and water, nickelous sulfateMass body volume concentrations is 300 grams per liters, and the mass body volume concentrations of nickel chloride is 40 grams per liters, the mass body volume concentrations of boric acidBe 40 grams per liters, the mass body volume concentrations of saccharin sodium is 5 mg/litre, and in bright nickel plating processing procedure, current density is 0.2Ampere/square decimeter, the temperature of the 3rd electronickelling solution is 45 degrees Celsius, pH value is 4.2;
7. the neodymium iron boron magnetic body that adopts deionized water to process bright nickel plating repeatedly cleans, and in cleaning process, is provided withUltrasonic Cleaning, ultrasonic power is 2000W, frequency is 40KHz.
In the present embodiment, pre-treatment adopts the conventional electroplating pretreatment process of the art, by sulfuric acid washing, waterWash, electrochemical deoiling and again washing step carry out pre-treatment.
Adopt the method for the present embodiment to 3.110 ± 0.010 millimeters of thickness, 4.67 square centimeters of end areas, girth 10.6Centimetre, the neodymium iron boron magnetic body product of profile tolerance 0.18, chamfering value 0.35 processes, neodymium iron boron magnetic body product concrete structureAs shown in Figure 1. By all identical neodymium iron boron magnetic body production sharing A group, B group and C groups of mentioned component, size and profileThree groups, carry out respectively electronickelling processing, the corresponding A of obtaining group, B group and C organize three groups of products after electronickelling. In phaseUnder condition, test respectively A group, B group and C and organize the bipolar flux value, 65 DEG C × 3 that fills of three groups of products after electronickellingHour attenuation losses rate, 150 DEG C × 1 hour ageing loss rate and dog bone effect value.
Bipolar method of testing of filling flux value is: first by magnet charger, product is carried out, after bipolar magnetizing, then using magnetic fluxInstrumentation examination flux value, the flux value that fluxmeter shows is the bipolar flux value that fills; The survey of 65 DEG C × 3 hours attenuation losses ratesMethod for testing is: the neodymium iron boron magnetic body after plating is undertaken, after bipolar magnetizing, recording flux value A1 by magnet charger, then putsIn drying oven 3 hours, in its stove, 65 DEG C of temperature were taken out and are again surveyed its magnetic flux from drying oven, record flux value A2,Its 65 DEG C × 3 hours attenuation losses rate=(A1-A2)/A1, loss late is less represents that its magnetic property is better; 150 DEG C × 1 is littleTime ageing loss rate: the neodymium iron boron magnetic body after plating is undertaken, after bipolar magnetizing, recording flux value B1, then by magnet chargerBe placed in drying oven interior 1 hour, 150 DEG C of temperature in its stove. After taking out, again carry out bipolar magnetizing, and survey its magnetic flux, surveyObtain flux value B2,150 DEG C × 1 hour ageing loss rate: (B1-B2)/B1, loss late is less represents that its magnetic property is better;Dog bone effect value: the difference of B point (being product point) finished size and A point (being product center portion) finished sizeBe called dog bone effect value, dog bone effect value is lower represents that its being uniformly distributed property of thickness of coating is better.
It is as shown in table 1 below that A group, B group and C organize after three groups of electronickellings the concrete data after neodymium iron boron magnetic body test:
Table 1
We can know analytical table 1: adopt the method for the present embodiment to process neodymium iron boron magnetic body, neodymium iron boron magnetic bodyThere is good magnetic property and being uniformly distributed property of thickness of coating.
Embodiment bis-: a kind of neodymium iron boron magnetic body method for electroplating nickel, comprises the following steps:
1. neodymium iron boron magnetic body is carried out to pre-treatment;
2. nickel preplating: the neodymium iron boron magnetic body after pre-treatment is put into the first electronickelling solution and carry out nickel preplating processing, timeBe 3500 seconds, wherein the first electronickelling solution is by nickelous sulfate, boric acid, succinate sodium salt, carboxyethyl sodium sulfonate and waterComposition, the mass body volume concentrations of nickelous sulfate is 250 grams per liters, the mass body volume concentrations of boric acid is 40 grams per liters, butanedioic acidThe mass body volume concentrations of ester sodium salt is 5 mg/litre, and the mass body volume concentrations of carboxyethyl sodium sulfonate is 5 mg/litre, preplatingIn nickel processing procedure, current density is 0.2 ampere/square decimeter, and the temperature of the first electronickelling solution is 45 degrees Celsius, pHValue is 4.1;
3. the neodymium iron boron magnetic body that adopts deionized water to process nickel preplating repeatedly cleans;
4. plate half light nickel: the neodymium iron boron magnetic body after cleaning is put into the second electronickelling solution and plate half light nickel processing, timeBetween be 4500 seconds, the second electronickelling solution is made up of nickelous sulfate, diammonium hydrogen citrate, boric acid, ammoniacal liquor and water, sulfuric acidThe mass body volume concentrations of nickel is 150 grams per liters, and the mass body volume concentrations of diammonium hydrogen citrate is 80 grams per liters, the matter of boric acidAmount volumetric concentration is 10 grams per liters, and the volumetric concentration of ammoniacal liquor is 20 milliliters/liter, current density in plating half light nickel processing procedureBe 0.2 ampere/square decimeter, the temperature of the second electronickelling solution is 45 degrees Celsius, and pH value is 6.5;
5. adopt deionized water repeatedly to clean the neodymium iron boron magnetic body that plates half light nickel and processed, in cleaning process, arrangeHave Ultrasonic Cleaning, ultrasonic power is 2000W, and frequency is 20KHz;
6. bright nickel plating: the neodymium iron boron magnetic body after cleaning is put into the 3rd electronickelling solution and carry out bright nickel plating processing, timeBetween be 3500 seconds, the 3rd electronickelling solution is made up of nickelous sulfate, nickel chloride, boric acid, saccharin sodium and water, nickelous sulfateMass body volume concentrations is 300 grams per liters, and the mass body volume concentrations of nickel chloride is 40 grams per liters, the mass body volume concentrations of boric acidBe 40 grams per liters, the mass body volume concentrations of saccharin sodium is 5 mg/litre, and in bright nickel plating processing procedure, current density is 0.2Ampere/square decimeter, the temperature of the 3rd electronickelling solution is 45 degrees Celsius, pH value is 4.2;
7. the neodymium iron boron magnetic body that adopts deionized water to process bright nickel plating repeatedly cleans, and in cleaning process, is provided withUltrasonic Cleaning, ultrasonic power is 2000W, frequency is 40KHz.
In the present embodiment, pre-treating technology comprises the following steps:
1.-1 pickling: adopt dilute nitric acid solution, as pickle, neodymium iron boron magnetic body is carried out to pickling;
1.-2 washings: the neodymium iron boron magnetic body after adopting deionized water to pickling repeatedly cleans, and is provided with in cleaning processUltrasonic Cleaning, ultrasonic power is 2000W, frequency is 20KHz;
1. the neodymium iron boron magnetic body after washing is put into electrolytic cell by-3 carries out electrolytic treatments, and the electrolytic treatments time is 200 seconds,Electrolyte is made up of NaOH, sodium carbonate and water, and the mass body volume concentrations of NaOH is 20 grams per liters, sodium carbonateMass body volume concentrations be 10 grams per liters, in electrolytic treatments process, current density is 0.2 ampere/square decimeter, electrolyteTemperature is 30 degrees Celsius;
1.-4 washings: the neodymium iron boron magnetic body after adopting deionized water to electrolysis repeatedly cleans, and is provided with in cleaning processUltrasonic Cleaning, ultrasonic power is 2000W, frequency is 20KHz.
In the method pair that adopts the present embodiment and embodiment mono-, the neodymium iron boron magnetic body product of same size is processed. By above-mentionedComposition, size and profile all identical neodymium iron boron magnetic body production sharing A group, B group and C are organized three groups, electroplate respectivelyNickel processing, the corresponding A of obtaining group, B group and C organize three groups of products after electronickelling. Under the same conditions, test respectively AGroup, B group and C organize three groups of products after electronickelling the bipolar flux value, 65 DEG C × 3 hours attenuation losses rates, 150 DEG C of filling× 1 hour ageing loss rate and dog bone effect value, method of testing is with embodiment mono-.
It is as shown in table 2 below that A group, B group and C organize after three groups of electronickellings the concrete data after neodymium iron boron magnetic body test:
Table 2
We can know analytical table 2: adopt the method for the present embodiment to process neodymium iron boron magnetic body, neodymium iron boron magnetic bodyThere is good magnetic property and being uniformly distributed property of thickness of coating.
Below embodiment mono-is detected to data mean value with embodiment bis-products and make contrast, concrete comparing result is as shown in table 3:
Table 3
| Project | Comparing result |
| The bipolar flux value that fills after plating | Embodiment bis-is higher by 0.2% than embodiment mono- |
| 65 DEG C × 3 hours attenuation losses ratios | Embodiment bis-is lower by 7.8% than embodiment mono- |
| 150 DEG C × 1 hour ageing loss ratio | Embodiment bis-is lower by 11.4% than embodiment mono- |
| Dog bone effect value | Embodiment bis-is identical with embodiment mono- |
From table 3 data we can find out, its decay of embodiment bis-and ageing loss ratio will be much smaller than embodiment mono-,Embodiment bis-magnetic properties are better than embodiment mono-thus, and embodiment mono-is suitable with embodiment bis-being uniformly distributed property of thickness of coating.We can know the pre-treating technology that adopts embodiment bis-analytical table 3, can reduce the magnetic property loss of neodymium iron boron magnetic body,Ensure that electronickelling neodymium iron boron magnetic body after treatment has good magnetic property.
Embodiment tri-: the present embodiment and embodiment bis-are basic identical, difference is only in the present embodiment, pre-treating technology bagDraw together following steps:
1.-1 pickling: adopt dilute nitric acid solution, as pickle, neodymium iron boron magnetic body is carried out to pickling;
1.-2 washings: the neodymium iron boron magnetic body after adopting deionized water to pickling repeatedly cleans, and is provided with in cleaning processUltrasonic Cleaning, ultrasonic power is 2000W, frequency is 60KHz;
1. the neodymium iron boron magnetic body after washing is put into electrolytic cell by-3 carries out electrolytic treatments, and the electrolytic treatments time is 450 seconds,Electrolyte is made up of NaOH, sodium carbonate and water, and the mass body volume concentrations of NaOH is 60 grams per liters, sodium carbonateMass body volume concentrations be 40 grams per liters, in electrolytic treatments process, current density is 0.7 ampere/square decimeter, electrolyteTemperature is 60 degrees Celsius;
1.-4 washings: the neodymium iron boron magnetic body after adopting deionized water to electrolysis repeatedly cleans, and is provided with in cleaning processUltrasonic Cleaning, ultrasonic power is 2000W, frequency is 60KHz.
In the method pair that adopts the present embodiment and embodiment mono-, the neodymium iron boron magnetic body product of same size is processed. By above-mentionedComposition, size and profile all identical neodymium iron boron magnetic body production sharing A group, B group and C are organized three groups, electroplate respectivelyNickel processing, the corresponding A of obtaining group, B group and C organize three groups of products after electronickelling. Under the same conditions, test respectively AGroup, B group and C organize three groups of products after electronickelling the bipolar flux value, 65 DEG C × 3 hours attenuation losses rates, 150 DEG C of filling× 1 hour ageing loss rate and dog bone effect value, method of testing is with embodiment mono-.
It is as shown in table 4 below that A group, B group and C organize after three groups of electronickellings the concrete data after neodymium iron boron magnetic body test:
Table 4
We can know analytical table 4: adopt the method for the present embodiment to process neodymium iron boron magnetic body, neodymium iron boron magnetic bodyThere is good magnetic property and being uniformly distributed property of thickness of coating.
Below embodiment mono-is detected to data mean value with embodiment three products and make contrast, concrete comparing result is as shown in table 5:
Table 5
| Project | Comparing result |
| The bipolar flux value that fills after plating | Embodiment tri-is higher by 0.5% than embodiment mono- |
| 65 DEG C × 3 hours attenuation losses ratios | Embodiment tri-is lower by 7.8% than embodiment mono- |
| 150 DEG C × 1 hour ageing loss ratio | Embodiment tri-is lower by 11.8% than embodiment mono- |
| Dog bone effect value | Embodiment tri-and the high 0.001mm of embodiment mono- |
From table 5 data we can find out, its decay of embodiment tri-and ageing loss ratio will be much smaller than embodiment mono-,Embodiment tri-magnetic properties are better than embodiment mono-thus, and the dog bone effect value of embodiment tri-is micro-higher than embodiment mono-, equally canSuitable to find out both being uniformly distributed property of thickness of coating. We can know the pre-treatment work that adopts embodiment tri-analytical table 5Skill, can reduce the magnetic property loss of neodymium iron boron magnetic body, ensures that electronickelling neodymium iron boron magnetic body after treatment has good magneticPerformance.
Embodiment tetra-: a kind of neodymium iron boron magnetic body method for electroplating nickel, comprises the following steps:
1. neodymium iron boron magnetic body is carried out to pre-treatment;
2. nickel preplating: the neodymium iron boron magnetic body after pre-treatment is put into the first electronickelling solution and carry out nickel preplating processing, timeBe 3500 seconds, wherein the first electronickelling solution is by nickelous sulfate, boric acid, succinate sodium salt, carboxyethyl sodium sulfonate and waterComposition, the mass body volume concentrations of nickelous sulfate is 220 grams per liters, the mass body volume concentrations of boric acid is 30 grams per liters, butanedioic acidThe mass body volume concentrations of ester sodium salt is 5 mg/litre, and the mass body volume concentrations of carboxyethyl sodium sulfonate is 5 mg/litre, preplatingIn nickel processing procedure, current density is 0.1 ampere/square decimeter, and the temperature of the first electronickelling solution is 40 degrees Celsius, pHValue is 4.5;
3. the neodymium iron boron magnetic body that adopts deionized water to process nickel preplating repeatedly cleans;
4. plate half light nickel: the neodymium iron boron magnetic body after cleaning is put into the second electronickelling solution and plate half light nickel processing, timeBetween be that 4500, the second electronickelling solution are made up of nickelous sulfate, diammonium hydrogen citrate, boric acid, ammoniacal liquor and water, nickelous sulfateMass body volume concentrations is 100 grams per liters, and the mass body volume concentrations of diammonium hydrogen citrate is 65 grams per liters, the mass body of boric acidVolume concentrations is 10 grams per liters, and the volumetric concentration of ammoniacal liquor is 20 milliliters/liter, and in plating half light nickel processing procedure, current density is 0.2Ampere/square decimeter, the temperature of the second electronickelling solution is 40 degrees Celsius, pH value is 7.0;
5. adopt deionized water repeatedly to clean the neodymium iron boron magnetic body that plates half light nickel and processed, in cleaning process, arrangeHave Ultrasonic Cleaning, ultrasonic power is 2000W, and frequency is 20KHz;
6. bright nickel plating: the neodymium iron boron magnetic body after cleaning is put into the 3rd electronickelling solution and carry out bright nickel plating processing,Time is 3500 seconds, and the 3rd electronickelling solution is made up of nickelous sulfate, nickel chloride, boric acid, saccharin sodium and water, nickelous sulfateMass body volume concentrations be 220 grams per liters, the mass body volume concentrations of nickel chloride is 20 grams per liters, the quality volume of boric acid is denseDegree is 30 grams per liters, and the mass body volume concentrations of saccharin sodium is 5 mg/litre, and in bright nickel plating processing procedure, current density is0.1 ampere/square decimeter, the temperature of the 3rd electronickelling solution is 40 degrees Celsius, and pH value is 4.8;
7. the neodymium iron boron magnetic body that adopts deionized water to process bright nickel plating repeatedly cleans, and in cleaning process, is provided withUltrasonic Cleaning, ultrasonic power is 2000W, frequency is 40KHz.
In the present embodiment, pre-treatment adopts the conventional electroplating pretreatment process of the art.
In the method pair that adopts the present embodiment and embodiment mono-, the neodymium iron boron magnetic body product of same size is processed. By above-mentionedComposition, size and profile all identical neodymium iron boron magnetic body production sharing A group, B group and C are organized three groups, electroplate respectivelyNickel processing, the corresponding A of obtaining group, B group and C organize three groups of products after electronickelling. Under the same conditions, test respectively AGroup, B group and C organize three groups of products after electronickelling the bipolar flux value, 65 DEG C × 3 hours attenuation losses rates, 150 DEG C of filling× 1 hour ageing loss rate and dog bone effect value, method of testing is with embodiment mono-.
It is as shown in table 6 below that A group, B group and C organize after three groups of electronickellings the concrete data after neodymium iron boron magnetic body test:
Table 6
We can know analytical table 6: adopt the method for the present embodiment to process neodymium iron boron magnetic body, neodymium iron boron magnetic bodyThere is good magnetic property and being uniformly distributed property of thickness of coating.
Embodiment five: the present embodiment and embodiment tetra-are basic identical, difference is only in the present embodiment, pre-treating technology bagDraw together following steps:
1.-1 pickling: adopt dilute nitric acid solution, as pickle, neodymium iron boron magnetic body is carried out to pickling;
1.-2 washings: the neodymium iron boron magnetic body after adopting deionized water to pickling repeatedly cleans, and is provided with in cleaning processUltrasonic Cleaning, ultrasonic power is 2000W, frequency is 45KHz;
1. the neodymium iron boron magnetic body after washing is put into electrolytic cell by-3 carries out electrolytic treatments, and the electrolytic treatments time is 200～450Second, electrolyte is made up of NaOH, sodium carbonate and water, and the mass body volume concentrations of NaOH is 45 grams per liters, carbonThe mass body volume concentrations of acid sodium is 25 grams per liters, and in electrolytic treatments process, current density is 0.5 ampere/square decimeter, electricitySeparating liquid temp is 45 degrees Celsius;
1.-4 washings: the neodymium iron boron magnetic body after adopting deionized water to electrolysis repeatedly cleans, and arranges in cleaning processHave Ultrasonic Cleaning, ultrasonic power is 2000W, and frequency is 45KHz.
In the method pair that adopts the present embodiment and embodiment mono-, the neodymium iron boron magnetic body product of same size is processed. By above-mentionedComposition, size and profile all identical neodymium iron boron magnetic body production sharing A group, B group and C are organized three groups, electroplate respectivelyNickel processing, the corresponding A of obtaining group, B group and C organize three groups of products after electronickelling. Under the same conditions, test respectively AGroup, B group and C organize three groups of products after electronickelling the bipolar flux value, 65 DEG C × 3 hours attenuation losses rates, 150 DEG C of filling× 1 hour ageing loss rate and dog bone effect value, method of testing is with embodiment mono-.
It is as shown in table 7 below that A group, B group and C organize after three groups of electronickellings the concrete data after neodymium iron boron magnetic body test:
Table 7
We can know analytical table 7: adopt the method for the present embodiment to process neodymium iron boron magnetic body, neodymium iron boron magnetic bodyThere is good magnetic property and being uniformly distributed property of thickness of coating.
Below embodiment tetra-is detected to data mean value with embodiment five products and make contrast, concrete comparing result is as shown in table 8:
Table 8
| Project | Comparing result |
| The bipolar flux value that fills after plating | Embodiment five is higher by 0.6% than embodiment tetra- |
| 65 DEG C × 3 hours attenuation losses ratios | Embodiment five is lower by 4.4% than embodiment tetra- |
| 150 DEG C × 1 hour ageing loss ratio | Embodiment five is lower by 3.3% than embodiment tetra- |
| Dog bone effect value | Embodiment five is than the low 0.001mm of embodiment tetra- |
From table 8 data we can find out, its decay of embodiment five and ageing loss ratio will be much smaller than embodiment tetra-,Embodiment five magnetic properties are better than embodiment tetra-thus, and the dog bone effect value of embodiment five is more lower slightly than embodiment tetra-, equally canSuitable to find out both being uniformly distributed property of thickness of coating. We can know the pre-treatment work that adopts embodiment five analytical table 8Skill, can reduce the magnetic property loss of neodymium iron boron magnetic body, ensures that electronickelling neodymium iron boron magnetic body after treatment has good magneticPerformance.
Embodiment six: a kind of neodymium iron boron magnetic body method for electroplating nickel, comprises the following steps:
1. neodymium iron boron magnetic body carries out pre-treatment;
2. nickel preplating: the neodymium iron boron magnetic body after pre-treatment is put into the first electronickelling solution and carry out nickel preplating processing, timeBe 3500 seconds, wherein the first electronickelling solution is by nickelous sulfate, boric acid, succinate sodium salt, carboxyethyl sodium sulfonate and waterComposition, the mass body volume concentrations of nickelous sulfate is 380 grams per liters, the mass body volume concentrations of boric acid is 60 grams per liters, butanedioic acidThe mass body volume concentrations of ester sodium salt is 20 mg/litre, and the mass body volume concentrations of carboxyethyl sodium sulfonate is 20 mg/litre, pre-In Nickel Plating Treatment process, current density is 0.6 ampere/square decimeter, and the temperature of the first electronickelling solution is 65 degrees Celsius,PH value is 3.8;
3. the neodymium iron boron magnetic body that adopts deionized water to process nickel preplating repeatedly cleans;
4. plate half light nickel: the neodymium iron boron magnetic body after cleaning is put into the second electronickelling solution and plate half light nickel processing, timeBetween be 4500 seconds, the second electronickelling solution is made up of nickelous sulfate, diammonium hydrogen citrate, boric acid, ammoniacal liquor and water, sulfuric acidThe mass body volume concentrations of nickel is 210 grams per liters, and the mass body volume concentrations of diammonium hydrogen citrate is 145 grams per liters, the matter of boric acidAmount volumetric concentration is 40 grams per liters, and the volumetric concentration of ammoniacal liquor is 60 milliliters/liter, current density in plating half light nickel processing procedureBe 0.7 ampere/square decimeter, the temperature of the second electronickelling solution is 65 degrees Celsius, and pH value is 5.7;
5. adopt deionized water repeatedly to clean the neodymium iron boron magnetic body that plates half light nickel and processed, in cleaning process, arrangeHave Ultrasonic Cleaning, ultrasonic power is 2000W, and frequency is 60KHz;
6. bright nickel plating: the neodymium iron boron magnetic body after cleaning is put into the 3rd electronickelling solution and carry out bright nickel plating processing, timeBetween be 3500 seconds, the 3rd electronickelling solution is made up of nickelous sulfate, nickel chloride, boric acid, saccharin sodium and water, nickelous sulfateMass body volume concentrations is 380 grams per liters, and the mass body volume concentrations of nickel chloride is 60 grams per liters, the mass body volume concentrations of boric acidBe 60 grams per liters, the mass body volume concentrations of saccharin sodium is 20 mg/litre, and in bright nickel plating processing procedure, current density is 0.6Ampere/square decimeter, the temperature of the 3rd electronickelling solution is 65 degrees Celsius, pH value is 3.8;
7. the neodymium iron boron magnetic body that adopts deionized water to process bright nickel plating repeatedly cleans, and in cleaning process, is provided withUltrasonic Cleaning, ultrasonic power is 2000W, frequency is 138KHz.
In the present embodiment, pre-treatment adopts the conventional electroplating pretreatment process of the art.
In the method pair that adopts the present embodiment and embodiment mono-, the neodymium iron boron magnetic body product of same size is processed. By above-mentionedComposition, size and profile all identical neodymium iron boron magnetic body production sharing A group, B group and C are organized three groups, electroplate respectivelyNickel processing, the corresponding A of obtaining group, B group and C organize three groups of products after electronickelling. Under the same conditions, test respectively AGroup, B group and C organize three groups of products after electronickelling the bipolar flux value, 65 DEG C × 3 hours attenuation losses rates, 150 DEG C of filling× 1 hour ageing loss rate and dog bone effect value, method of testing is with embodiment mono-.
It is as shown in table 9 below that A group, B group and C organize after three groups of electronickellings the concrete data after neodymium iron boron magnetic body test:
Table 9
We can know analytical table 9: adopt the method for the present embodiment to process neodymium iron boron magnetic body, neodymium iron boron magnetic bodyThere is good magnetic property and being uniformly distributed property of thickness of coating.
Embodiment seven: the present embodiment and embodiment six are basic identical, difference is only in the present embodiment, pre-treating technology bagDraw together following steps:
1.-1 pickling: adopt dilute nitric acid solution, as pickle, neodymium iron boron magnetic body is carried out to pickling;
1.-2 washings: the neodymium iron boron magnetic body after adopting deionized water to pickling repeatedly cleans, and is provided with in cleaning processUltrasonic Cleaning, ultrasonic power is 2000W, frequency is 45KHz;
1. the neodymium iron boron magnetic body after washing is put into electrolytic cell by-3 carries out electrolytic treatments, and the electrolytic treatments time is 200～450Second, electrolyte is made up of NaOH, sodium carbonate and water, and the mass body volume concentrations of NaOH is 45 grams per liters, carbonThe mass body volume concentrations of acid sodium is 25 grams per liters, and in electrolytic treatments process, current density is 0.5 ampere/square decimeter, electricitySeparating liquid temp is 45 degrees Celsius;
1.-4 washings: the neodymium iron boron magnetic body after adopting deionized water to electrolysis repeatedly cleans, and arranges in cleaning processHave Ultrasonic Cleaning, ultrasonic power is 2000W, and frequency is 45KHz.
In the method pair that adopts the present embodiment and embodiment mono-, the neodymium iron boron magnetic body product of same size is processed. By above-mentionedComposition, size and profile all identical neodymium iron boron magnetic body production sharing A group, B group and C are organized three groups, electroplate respectivelyNickel processing, the corresponding A of obtaining group, B group and C organize three groups of products after electronickelling. Under the same conditions, test respectively AGroup, B group and C organize three groups of products after electronickelling the bipolar flux value, 65 DEG C × 3 hours attenuation losses rates, 150 DEG C of filling× 1 hour ageing loss rate and dog bone effect value, method of testing is with embodiment mono-.
It is as shown in table 10 below that A group, B group and C organize after three groups of electronickellings the concrete data after neodymium iron boron magnetic body test:
Table 10
We can know analytical table 10: adopt the method for the present embodiment to process neodymium iron boron magnetic body, neodymium-iron-boronBody has good magnetic property and being uniformly distributed property of thickness of coating.
Below embodiment six is detected to data mean value with embodiment seven products and make contrast, concrete comparing result is as table 11Show:
Table 11
| Project | Comparing result |
| The bipolar flux value that fills after plating | Embodiment seven is identical with embodiment six |
| 65 DEG C × 3 hours attenuation losses ratios | Embodiment seven is lower by 2.3% than embodiment six |
| 150 DEG C × 1 hour ageing loss ratio | Embodiment seven is lower by 0.4% than embodiment six |
| Dog bone effect value | Embodiment seven is identical with embodiment six |
From table 11 data we can find out, its decay of embodiment seven and ageing loss ratio will be slightly less than embodiment six,Embodiment seven magnetic properties are better than embodiment six thus, and the dog bone effect value of embodiment seven is identical with embodiment six, equally canSuitable to find out both being uniformly distributed property of thickness of coating. We can know the pre-treatment that adopts embodiment seven analytical table 11Technique, can reduce the magnetic property loss of neodymium iron boron magnetic body, ensures that electronickelling neodymium iron boron magnetic body after treatment has preferablyMagnetic property.
Adopt the electronickelling technique of existing neodymium iron boron magnetic body and existing conventional pre-treating technology to phase in above-described embodimentThe neodymium iron boron magnetic body of same specification carries out electronickelling processing, and neodymium iron boron magnetic body product is also divided into A group, B group and C group threeGroup is carried out respectively electronickelling processing, and the corresponding A of obtaining group, B group and C organize three groups of neodymium iron boron magnetic body products after electronickelling.Under the same conditions, the bipolar flux value, 65 DEG C of filling of testing respectively that A group, B group and C organize three groups of products after electronickelling× 3 hours attenuation losses rates, 150 DEG C × 1 hour ageing loss rate and dog bone effect value, method of testing is with embodiment mono-.
Adopt A group, B group and the C of the electronickelling PROCESS FOR TREATMENT of existing neodymium iron boron magnetic body to organize neodymium iron after three groups of electronickellingsConcrete data after boron magnet test are as shown in table 12 below:
Table 12
The data of the data of table 12 and embodiment mono-to embodiment seven are contrasted, and we can know existing electronickellingThe neodymium iron boron magnetic body that method obtains bipolar fills flux value and is less than the bipolar of neodymium iron boron magnetic body that method of the present invention obtains and fillsFlux value, and 65 DEG C × 3 hours attenuation losses ratios and 150 DEG C × 1 hour ageing loss rate are all much larger than of the present inventionThe bipolar flux value that fills of the neodymium iron boron magnetic body that method obtains, hence one can see that, the neodymium iron boron magnetic body of method processing of the present inventionMagnetic property is significantly improved; The dog bone effect value of the neodymium iron boron magnetic body that existing method for electroplating nickel obtains is much larger than thisThe dog bone effect value of the neodymium iron boron magnetic body that the method for invention obtains, hence one can see that, the neodymium-iron-boron of method processing of the present inventionThe being uniformly distributed property of thickness of coating of body is significantly improved.
Claims (2)
1. a neodymium iron boron magnetic body method for electroplating nickel, is characterized in that comprising the following steps:
1. neodymium iron boron magnetic body is carried out to pre-treatment;
2. nickel preplating: the neodymium iron boron magnetic body after pre-treatment is put into the first electronickelling solution and carry out nickel preplating processing, timeBe 2500～5500 seconds, wherein the first electronickelling solution is by nickelous sulfate, boric acid, succinate sodium salt, carboxyethyl sulfonic acidSodium and water composition, the mass body volume concentrations of nickelous sulfate is 220～380 grams per liters, the mass body volume concentrations of boric acid is 30～60Grams per liter, the mass body volume concentrations of succinate sodium salt is 5～20 mg/litre, the mass body volume concentrations of carboxyethyl sodium sulfonateBe 5～20 mg/litre, in nickel preplating processing procedure, current density is 0.1～0.6 ampere/square decimeter, and first electroplatesThe temperature of nickel solution is 40～65 degrees Celsius, and pH value is 3.5～4.8;
3. the neodymium iron boron magnetic body that adopts deionized water to process nickel preplating repeatedly cleans;
4. plate half light nickel: the neodymium iron boron magnetic body after cleaning is put into the second electronickelling solution and plate half light nickel processing, timeBetween be 3500～6500 seconds, the second electronickelling solution is made up of nickelous sulfate, diammonium hydrogen citrate, boric acid, ammoniacal liquor and water,The mass body volume concentrations of nickelous sulfate is 100～210 grams per liters, and the mass body volume concentrations of diammonium hydrogen citrate is 65～145 grams/ liter, the mass body volume concentrations of boric acid is 10～40 grams per liters, the volumetric concentration of ammoniacal liquor is 20～60 milliliters/liter, plating halfIn light nickel processing procedure, current density is 0.2～0.7 ampere/square decimeter, and the temperature of the second electronickelling solution is 40～65Degree Celsius, pH value is 5.5～7.5;
5. adopt deionized water repeatedly to clean the neodymium iron boron magnetic body that plates half light nickel and processed, in cleaning process, arrangeHave Ultrasonic Cleaning, ultrasonic power is 2000W, and frequency is 20～60KHz;
6. bright nickel plating: the neodymium iron boron magnetic body after cleaning is put into the 3rd electronickelling solution and carry out bright nickel plating processing, timeBetween be 2500～5500 seconds, the 3rd electronickelling solution is made up of nickelous sulfate, nickel chloride, boric acid, saccharin sodium and water, sulphurThe mass body volume concentrations of acid nickel is 220～380 grams per liters, and the mass body volume concentrations of nickel chloride is 20～60 grams per liters, boronThe mass body volume concentrations of acid is 30～60 grams per liters, and the mass body volume concentrations of saccharin sodium is 5～20 mg/litre, and light-plated is brightIn nickel processing procedure, current density is 0.1～0.6 ampere/square decimeter, and the temperature of the 3rd electronickelling solution is 40～65Degree Celsius, pH value is 3.5～4.8;
7. the neodymium iron boron magnetic body that adopts deionized water to process bright nickel plating repeatedly cleans, and in cleaning process, is provided withUltrasonic Cleaning, ultrasonic power is 2000W, frequency is 40～138KHz.
2. neodymium iron boron magnetic body method for electroplating nickel according to claim 1, is characterized in that described pre-treating technology bagDraw together following steps:
1.-1 pickling: adopt dilute nitric acid solution, as pickle, neodymium iron boron magnetic body is carried out to pickling;
1.-2 washings: the neodymium iron boron magnetic body after adopting deionized water to pickling repeatedly cleans, and is provided with in cleaning processUltrasonic Cleaning, ultrasonic power is 2000W, frequency is 20～60KHz;
1. the neodymium iron boron magnetic body after washing is put into electrolytic cell by-3 carries out electrolytic treatments, and the electrolytic treatments time is 200～450Second, electrolyte is made up of NaOH, sodium carbonate and water, and the mass body volume concentrations of NaOH is 20～60 grams per liters,The mass body volume concentrations of sodium carbonate is 10～40 grams per liters, in electrolytic treatments process current density be 0.2～0.7 ampere/flatSide's decimetre, electrolyte temperature is 30～60 degrees Celsius;
1.-4 washings: the neodymium iron boron magnetic body after adopting deionized water to electrolysis repeatedly cleans, and arranges in cleaning processHave Ultrasonic Cleaning, ultrasonic power is 2000W, and frequency is 20～60KHz.
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| CN105714293B (en) * | 2014-12-04 | 2018-12-21 | 安泰科技股份有限公司 | It is a kind of to have both high magnetic conduction and highly conductive composite material and preparation method |
| CN104789997A (en) * | 2015-04-27 | 2015-07-22 | 南京宁美表面技术有限公司 | Pearl nickel electroplating additive, pearl nickel electroplating solution and electroplating method |
| CN105220194A (en) * | 2015-10-16 | 2016-01-06 | 宁波韵升磁体元件技术有限公司 | A kind of method for electroplating nickel of neodymium iron boron thin slice magnet steel product |
| CN107604407A (en) * | 2017-10-31 | 2018-01-19 | 宁波和勤化学有限公司 | A kind of Nd-Fe-B magnet steel electroplating technology |
| CN108109834A (en) * | 2017-12-20 | 2018-06-01 | 宁波市鄞州智伴信息科技有限公司 | Strong permanent magnetism material formula of a kind of corrosion resistance and preparation method thereof |
| CN111334825B (en) * | 2018-12-19 | 2021-05-25 | 贵州振华群英电器有限公司（国营第八九一厂） | Sulfate system deep hole nickel plating additive, preparation method and electroplating process |
| CN110592623B (en) * | 2019-09-05 | 2021-01-05 | 宁波韵升股份有限公司 | Formula and method of nickel electroplating solution for improving uniform distribution of neodymium iron boron magnet coating |
| CN114908385B (en) * | 2022-06-08 | 2024-03-29 | 包头市英思特稀磁新材料股份有限公司 | Method for reducing hydrogen permeation damage of neodymium iron boron in acid nickel electroplating process |
| CN116005157B (en) * | 2022-12-13 | 2023-12-19 | 苏州圆格电子有限公司 | Neodymium iron boron surface pretreatment method and system |
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