CN105369226A - Chemical nickel phosphor plating solution for surface acidity of sintered NdFeB magnet, and nickel phosphor plating process - Google Patents
Chemical nickel phosphor plating solution for surface acidity of sintered NdFeB magnet, and nickel phosphor plating process Download PDFInfo
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Abstract
The invention relates to a chemical nickel phosphor plating solution for surface acidity of a sintered NdFeB magnet. The pH value of the chemical nickel phosphor plating solution is 4.5 to 5.0, and the chemical nickel phosphor plating solution comprises dissoluble nickel salt, a reducing agent, a composite complex agent, a buffer agent, a promoter and a stabilizer. The nickel phosphor plating process comprises the following steps: (1), carrying out ultrasonic acid pickling on the sintered NdFeB magnet for 20 to 40s, then carrying out ultrasonic water washing and regular water washing; (2), under a temperature of 55 to 60 DEG C, carrying out ultrasonic alkaline washing for 5 to 12 min, then carrying out ultrasonic water washing and regular water washing; (3), carrying out ultrasonic activation for 20 to 40s at a room temperature; and (4), placing into the nickel phosphor plating solution, carrying out ultrasonic plating for 60 to 180 min, and then carrying out water washing and drying. The nickel phosphor plating solution is environment friendly and has less pollution to the environment, an obtained clad layer is even in thickness, the porosity is low, magnetism loss is avoided, and corrosion resistance is excellent; and the nickel phosphor plating process is simple, the cost is low, and the binding force of the clad layer and a basal body is strong.
Description
Technical field
The present invention relates to a kind of nickel plating phosphorus solution and Ni-P-plating technique thereof, be specifically related to a kind of Sintered NdFeB magnet Acid electroless nickel-phosphorus plating solution and Ni-P-plating technique thereof.
Background technology
Third generation sintered neodymium iron boron material has the excellent performance such as magnetic property, mechanical property, good workability because of it, industrially obtains a wide range of applications.But, due to the Chemical Composition of sintered Nd-Fe-B magnetic material and the singularity of preparation technology, make it have some characteristic, if the nd-fe-b permanent magnetic alloy after sintering is polyphase structure structure, the resistance of oxidation of each phase is different with corrosion resisting property, and rich neodymium phase active in material, boron-rich phase are easily and principal phase Nd
2fe
14b forms galvanic cell, produces intergranular corrosion; Sintered Nd-Fe-B magnetic material surface porosity porous, coarse injustice that compacting sintering is shaping, there is micro-pore and cavity in inside, easily oxygen uptake makes rare earth element be oxidized in an atmosphere, destroys alloy compositions; And sintered neodymium iron boron material is containing the extremely strong neodymium of 1/3 chemically reactive of having an appointment, unstable chemcial property, and the rich neodymium phase wherein contained and principal phase have strong hydrogen-absorbing ability, easily produce and inhale hydrogen-type corrosion.Just because of these characteristics, cause Sintered NdFeB magnet that burn into oxidation very easily occurs in environment for use and from phenomenons such as efflorescence, therefore, surfacecti proteon process must be carried out to neodymium-iron-boron magnetic material.
At present, sintered Nd-Fe-B magnetic material surface treatment generally adopts the methods such as plating, electroless plating, chemical transformation film, electrophoresis and spraying, wherein, the coating obtained by Sintered NdFeB magnet chemical nickel phosphorus plating technology evenly, fine and close, hardness is high, corrosion resisting property and wear resisting property excellent, plating solution environmental protection, advantage of lower cost.Current chemical nickel phosphorus plating method has acidity, neutrality and alkaline chemical nickel-plating method, and wherein, it is low that acid chemical plating nickel phosphorus method can obtain porosity, and compactness is good, and phosphorus content is higher, the coating of excellent corrosion-proof performance.As CN101922608A discloses a kind of nickel-phosphorus alloy steel bottle and plating method thereof, it adopts the method for acid chemical plating nickel phosphorus, plating solution pH is 4.5 ~ 5.5, obtain and the amorphous nickel that matrix steel cylinder bonding force is good, thickness is even, corrosion resistance is excellent-phosphorus preservative coat on steel cylinder surface, but because the pH value of plating solution is too low, the corrodibility of plating solution to matrix NdFeB material is strong, cause the bonding force of coating and matrix NdFeB material poor, still can not directly plating on NdFeB material.At present, main employing preplating alkaline chemical nickel-plating, multilayer coating bottoming and the phosphatization pre-treatment etc. such as plating ambrose alloy, rotproofing is carried out again in conjunction with acid chemical nickel phosphorus plating, as the people such as Wu Xiuzhen pass through more acid and alkaline coating to the impact of permanent magnet material antiseptic property, wherein acid chemical plating liquid can not directly plating on sintered neodymium iron boron material, alkali electroless plating solution can obtain good coating on Nd-Fe-B matrix, but compared with alkaline coating, with alkaline coating for bottom, acid coating be the compound coating of top layer have better anti-corrosion effect (Wu Xiuzhen etc. Electroless Ni-P Alloy on Sintered Nd-Fe-B Permanent. Institutes Of Technology Of Taiyuan's journal, 34th volume the 6th phase, in November, 2003).But this complex process, cost is higher, and environmental pollution is larger.The people such as Yang Peiyan disclose the performance study of sintered Nd-Fe-B permanent magnet secondary Electroless Plating of Ni-P Alloy coating, adopt the bottoming of ultrasonic alkaline chemical nickel phosphorus plating, impose the acid chemical plating nickel-phosphorus alloy of secondary again, obtain that porosity is low, the alloy layer of excellent corrosion-proof performance (Yang Peiyan etc. Nd-Fe-B permanent magnet secondary Electroless Plating of Ni-P Alloy coating performance is studied. plating and finish, 30th volume the 12nd phase, in December, 2008).But this complex process, cost is higher, and environmental pollution is larger.
At present, people have started to have carried out preliminary study to the protection of chemical nickel phosphorus plating technology in neodymium-iron-boron surface.As CN100402698C discloses a kind of chemical nickel and phosphor plating method of Nd-Fe-Bo permanent magnet material, adopt electroless plating of pove sealing to thicken neodymium iron boron sealing of hole and neutral chemical plating and block, then carry out the chemical nickel phosphorus plating of acid high phosphorus chemical plating, finally impose passivation aftertreatment.But, in its neutral electroless plating and acid high phosphorus chemical plating liquid, contain toxic heavy metal ion Pb
2+, and adopting sexavalent chrome to carry out Passivation Treatment, its plating solution and technique are not environmentally, big for environment pollution, and operation is loaded down with trivial details, increase artificial and production cost.
Summary of the invention
Technical problem to be solved by this invention is, overcome prior art exist above-mentioned defect, provide a kind of coating and basal body binding force good, coating porosity is low, compactness is good, and phosphorus content is higher, the Sintered NdFeB magnet Acid electroless nickel-phosphorus plating solution of excellent corrosion-proof performance.
The technical problem that the present invention will solve further is, overcomes the above-mentioned defect that prior art exists, and provide a kind of technique simple, cost is low, environment friendly and pollution-free Acid electroless nickel-phosphorus plating technique.
The technical solution adopted for the present invention to solve the technical problems is as follows: a kind of Sintered NdFeB magnet Acid electroless nickel-phosphorus plating solution, and the pH value of described nickel plating phosphorus solution is 4.5 ~ 5.0, and it consists of:
Soluble nickel salt 25 ~ 28g/L,
Reductive agent 18 ~ 28g/L,
Compound complex agent 38 ~ 50g/L,
Buffer reagent 20 ~ 32g/L,
Promotor 0.5 ~ 1.5g/L,
Stablizer 1 ~ 3mg/L.
Further, the compound method of described nickel plating phosphorus solution is: according to the mass ratio of solute in nickel plating phosphorus solution, respectively compound complex agent is added water together with buffer reagent and heating for dissolving, soluble nickel salt is dissolved in water, then these two kinds of solution are mixed and stir, be denoted as solution A, again reductive agent is dissolved in water, then slowly pours in solution A while stirring, stir, be denoted as solution B, promotor and stablizer are dissolved in water, slowly pour in solution B, in the process of constant volume, use ammoniacal liquor adjust ph.In practical application in industry, the reagent purity used due to preparation nickel plating phosphorus solution mostly is technical grade, containing impurity, impurity in solution likely becomes the active particle of electroless deposition, then the self-catalyzed reaction of plating solution is caused, affect work-ing life and the coating performance of plating solution, so need to filter prepared solution, to remove insoluble impurity.
Further, described soluble nickel salt is single nickel salt; Described reductive agent is inferior sodium phosphate; Described compound complex agent is one or more in tartrate, succinic acid or lactic acid, and wherein, when tartrate and succinic acid are as compound complex agent, the concentration of nickel plating phosphorus solution unresolvable tartaric acid is 35 ~ 42g/L, and the concentration of succinic acid is 4 ~ 8g/L; Described buffer reagent is sodium acetate; Described promotor is Sodium Fluoride; Described stablizer is thiocarbamide or Potassium Iodate.
The present invention solves the technical scheme that its technical problem adopts further: a kind of Acid electroless nickel-phosphorus plating technique, comprises the following steps:
(1) ultrasonic pickling: Sintered NdFeB magnet is placed in pickle solution, at room temperature, ultrasonic pickling 20 ~ 40s, then through ultrasonic washing, conventional water wash, obtains pickling Sintered NdFeB magnet;
(2) ultrasonic alkali cleaning oil removing: step (1) gained pickling Sintered NdFeB magnet is placed in alkaline wash, at 55 ~ 60 DEG C, ultrasonic alkali cleaning oil removing 5 ~ 12min, then through ultrasonic washing, conventional water wash, obtains alkali cleaning Sintered NdFeB magnet;
(3) ultrasonic activation: step (2) gained alkali cleaning Sintered NdFeB magnet is placed in activation solution, at room temperature, ultrasonic activation 20 ~ 40s, obtains activated sintering neodymium iron boron magnetic body;
(4) ultrasonic chemistry: step (3) gained activated sintering neodymium iron boron magnetic body is placed in described Sintered NdFeB magnet Acid electroless nickel-phosphorus plating solution, ultrasonic plating 60 ~ 180min, washing, dries up.
Further, in step (4), the temperature of described ultrasonic plating is 80 ~ 90 DEG C.If the too low plating speed of plating temperature is too slow, affect the bonding force of coating and matrix, even plating solution not plating, if plating temperature is too high, plating speed too soon, easily there is self-decomposition in plating solution instability, affects plating solution work-ing life.Ultrasonic plating utilizes hyperacoustic impact and concussion effect, accelerate Sintered NdFeB magnet surface and chemical reaction occurs, improve sedimentation velocity, and the foaming in cling matrix surface and space is discharged in time, the combination of the aeration coating remained can be avoided to make coating peeling on the one hand, on the other hand, plating solution can enter in surface pore in time, fully, form even, fine and close, imporous coating, improve the bonding force of coating and matrix.Ultrasonic nickel plating phosphorus solves the problem that acid chemical plating nickel-phosphorus alloy coating technology can not directly apply to Sintered NdFeB magnet.
Further, in step (1), consisting of of described pickle solution: nitric acid 30 ~ 50mL/L, thiocarbamide 0.5 ~ 0.8g/L.Pickling can remove the black oxide film on sintered NdFeB black-film surface, obtains the matrix on even, careful silvery white surface.
Further, in step (2), consisting of of described alkaline wash: sodium hydroxide 8 ~ 10g/L, 12 hypophosphite monohydrate trisodium 60 ~ 80g/L, sodium carbonate 40 ~ 60g/L, and with pH value to 9 ~ 10 of formic acid regulator solution.Alkali cleaning can remove the greasy dirt, dirt etc. that sintering neodymium boron magnet surface adheres to, to obtain clean matrix surface.Formic acid for adjust ph has coordination to neodymium ion, can slow down the corrosion of alkaline wash to matrix.
Further, in step (1), (2), the time of described ultrasonic washing is 1 ~ 3min.Described conventional water wash comprises tap water and deionization washing.The object of washing removes the acid/alkaline wash of Sintered NdFeB magnet surface residual, avoids affecting subsequent operations.
Further, in step (3), described activation solution is the glacial acetic acid solution of 100 ~ 200mL/L.Activation thoroughly can remove the very thin oxide film in Sintered NdFeB magnet surface, thorough exposed matrix surface.Compared with traditional activating process, glacial acetic acid activating process is gentle, environmentally friendly, effectively can remove the oxide film of surface residual, can not produce excessive erosion to Sintered NdFeB magnet, glacial acetic acid is little to plating solution interference, without the need to cleaning after activation, directly enter groove, keep matrix surface moisture film to present low ph value, prevent matrix to be oxidized, affect the bonding force of coating and matrix.Selecting the concentration of glacial acetic acid to be 100 ~ 200mL/L is because if concentration is too low, soak time is long, does not reach desirable activation effect, if concentration is too high, easily produce excessive erosion to matrix, soak time is wayward.
Further, in step (1) ~ (4), the frequency of described supersound process is 35 ~ 45kHz, and power is 100 ~ 250W.In pretreatment process, adopt ultrasonic assistant to clean, be utilize hyperacoustic cavatition thoroughly to clean the oxide film of Sintered NdFeB magnet inner aperture, greasy dirt and debris.
Advantage of the present invention and effect:
(1) chemical nickel-plating solution of the present invention adopts acid formula, the high P non-crystalline coating of easy acquisition, and the reagent environmental protection in nickel plating phosphorus liquid, environmental pollution is little, and gained coating thickness is even, and porosity is low, there is excellent corrosion resistance nature, and coating is magnetic conduction not, be conducive to the maintenance of magnetic field magnetic performance, nonmagnetic rate of loss;
(2) Ni-P-plating technique of the present invention uses ultrasonic wave added to contribute to the oxide film and the impurity that thoroughly clean Sintered NdFeB magnet inner aperture in pre-treatment, uses ultrasonic wave added then to contribute to improving the bonding force of coating and matrix in electroless plating plating process;
(3) Ni-P-plating technique of the present invention does not need special pre-treatment and pre-plating process, simplifies technical process, reduces production cost, is easy to control of industrialization.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
The trade mark of the Sintered NdFeB magnet black-film that the embodiment of the present invention uses is N38M, and dimensions is F10mm × 10mm × 5mm; Other chemical reagent used is analytical pure, if no special instructions, is all obtained by routine business approach.
embodiment 1
The compound method of nickel plating phosphorus solution is: by 40g tartrate, and 6g succinic acid adds water and heating for dissolving together with 30g sodium acetate, is dissolved in water by 26g single nickel salt, then these two kinds of solution mixed and stir, being denoted as solution A, then 26g inferior sodium phosphate is dissolved in water, then slowly pour into while stirring in solution A, stir, be denoted as solution B, 1g Sodium Fluoride and 1mg thiocarbamide are dissolved in water, slowly pour in solution B, be settled in the process of 1L, by ammoniacal liquor adjust ph to 4.8.
A kind of Sintered NdFeB magnet Acid electroless nickel-phosphorus plating solution, the pH value of described nickel plating phosphorus solution is 4.8, and it consists of:
Single nickel salt 26g/L,
Inferior sodium phosphate 26g/L,
Tartrate 40g/L,
Succinic acid 6g/L,
Sodium acetate 30g/L,
Sodium Fluoride 1g/L,
Thiocarbamide 1mg/L.
Acid electroless nickel-phosphorus plating technique:
(1) ultrasonic pickling: Sintered NdFeB magnet is placed in pickle solution (nitric acid 30mL/L, thiocarbamide 0.5g/L), at room temperature, ultrasonic pickling 30s, then through ultrasonic washing 1min, then first tap water, then deionization is washed, and obtains pickling Sintered NdFeB magnet;
(2) ultrasonic alkali cleaning oil removing: step (1) gained pickling Sintered NdFeB magnet is placed in alkaline wash (sodium hydroxide 9g/L, 12 hypophosphite monohydrate trisodium 70g/L, sodium carbonate 50g/L, and by the pH value to 9.69 of formic acid regulator solution) in, at 55 DEG C, ultrasonic alkali cleaning oil removing 10min, again through ultrasonic washing 2min, then first tap water, then deionization is washed, and obtains alkali cleaning Sintered NdFeB magnet;
(3) ultrasonic activation: glacial acetic acid solution step (2) gained alkali cleaning Sintered NdFeB magnet being placed in 150mL/L, at room temperature, ultrasonic activation 30s, obtains activated sintering neodymium iron boron magnetic body;
(4) ultrasonic chemistry: step (3) gained activated sintering neodymium iron boron magnetic body is placed in described Sintered NdFeB magnet Acid electroless nickel-phosphorus plating solution, at 82 DEG C, ultrasonic plating 60min, washing, dries up.
In step (1) ~ (4), the frequency of described supersound process is 35kHz, and power is 140W.
The present embodiment gained nickel-phosphorus alloy coating thickness is 8 μm, and thickness is even, and porosity is 4/cm
2, magnetic loss rate is 0%; This nickel-phosphorus alloy coating evenly, be silvery white in color metal color, and by observation by light microscope, coating is without foaming and the defect such as to peel off, coating light, bath stability; Carry out bonding force test according to the thermal shock test specified in standard GB/T5270-2005 (temperature is 300 DEG C, insulation 1h), coating is without peeling, obscission, and coating is combined with matrix well; Under the neutral salt spray condition specified according to standard GB/T10125-1997 " artificial atmosphere corrosion test-salt-fog test ", (5wt%NaCl, 35 ± 1 DEG C) are tested, and the magnet resistance to neutral salt spray time reaches 120h.
embodiment 2
The compound method of nickel plating phosphorus solution is: by 42g tartrate, and 8g succinic acid adds water and heating for dissolving together with 32g sodium acetate, is dissolved in water by 28g single nickel salt, then these two kinds of solution mixed and stir, being denoted as solution A, then 28g inferior sodium phosphate is dissolved in water, then slowly pour into while stirring in solution A, stir, be denoted as solution B, 1.5g Sodium Fluoride and 3mg thiocarbamide are dissolved in water, slowly pour in solution B, be settled in the process of 1L, by ammoniacal liquor adjust ph to 4.6.
A kind of Sintered NdFeB magnet Acid electroless nickel-phosphorus plating solution, the pH value of described nickel plating phosphorus solution is 4.6, and it consists of:
Single nickel salt 28g/L,
Inferior sodium phosphate 28g/L,
Tartrate 42g/L,
Succinic acid 8g/L,
Sodium acetate 32g/L,
Sodium Fluoride 1.5g/L,
Thiocarbamide 3mg/L.
Acid electroless nickel-phosphorus plating technique:
(1) ultrasonic pickling: Sintered NdFeB magnet is placed in pickle solution (nitric acid 40mL/L, thiocarbamide 0.6g/L), at room temperature, ultrasonic pickling 30s, then through ultrasonic washing 1min, then first tap water, then deionization is washed, and obtains pickling Sintered NdFeB magnet;
(2) ultrasonic alkali cleaning oil removing: step (1) gained pickling Sintered NdFeB magnet is placed in alkaline wash (sodium hydroxide 10g/L, 12 hypophosphite monohydrate trisodium 80g/L, sodium carbonate 60g/L, and by the pH value to 10 of formic acid regulator solution) in, at 58 DEG C, ultrasonic alkali cleaning oil removing 8min, again through ultrasonic washing 3min, then first tap water, then deionization is washed, and obtains alkali cleaning Sintered NdFeB magnet;
(3) ultrasonic activation: glacial acetic acid solution step (2) gained alkali cleaning Sintered NdFeB magnet being placed in 200mL/L, at room temperature, ultrasonic activation 20s, obtains activated sintering neodymium iron boron magnetic body;
(4) ultrasonic chemistry: step (3) gained activated sintering neodymium iron boron magnetic body is placed in described Sintered NdFeB magnet Acid electroless nickel-phosphorus plating solution, at 90 DEG C, ultrasonic plating 120min, washing, dries up.
In step (1) ~ (4), the frequency of described supersound process is 40kHz, and power is 240W.
The present embodiment gained nickel-phosphorus alloy coating thickness is 18 μm, and thickness is even, and porosity is 3/cm
2, magnetic loss rate is 0%; This nickel-phosphorus alloy coating evenly, be silvery white in color metal color, and by observation by light microscope, coating is without foaming and the defect such as to peel off, coating light, bath stability; Carry out bonding force test according to the thermal shock test specified in standard GB/T5270-2005 (temperature is 300 DEG C, insulation 1h), coating is without peeling, obscission, and coating is combined with matrix well; Under the neutral salt spray condition specified according to standard GB/T10125-1997 " artificial atmosphere corrosion test-salt-fog test ", (5wt%NaCl, 35 ± 1 DEG C) are tested, and the magnet resistance to neutral salt spray time reaches 214h.
embodiment 3
The compound method of nickel plating phosphorus solution is: by 35g tartrate, and 4g succinic acid adds water and heating for dissolving together with 25g sodium acetate, is dissolved in water by 25g single nickel salt, then these two kinds of solution mixed and stir, being denoted as solution A, then 20g inferior sodium phosphate is dissolved in water, then slowly pour into while stirring in solution A, stir, be denoted as solution B, 0.5g Sodium Fluoride and 1mg thiocarbamide are dissolved in water, slowly pour in solution B, be settled in the process of 1L, by ammoniacal liquor adjust ph to 5.0.
A kind of Sintered NdFeB magnet Acid electroless nickel-phosphorus plating solution, the pH value of described nickel plating phosphorus solution is 5.0, and it consists of:
Single nickel salt 25g/L,
Inferior sodium phosphate 20g/L,
Tartrate 35g/L,
Succinic acid 4g/L,
Sodium acetate 25g/L,
Sodium Fluoride 0.5g/L,
Thiocarbamide 1mg/L.
Acid electroless nickel-phosphorus plating technique:
(1) ultrasonic pickling: Sintered NdFeB magnet is placed in pickle solution (nitric acid 50mL/L, thiocarbamide 0.8g/L), at room temperature, ultrasonic pickling 20s, then through ultrasonic washing 2min, then first tap water, then deionization is washed, and obtains pickling Sintered NdFeB magnet;
(2) ultrasonic alkali cleaning oil removing: step (1) gained pickling Sintered NdFeB magnet is placed in alkaline wash (sodium hydroxide 8g/L, 12 hypophosphite monohydrate trisodium 60g/L, sodium carbonate 40g/L, and by the pH value to 9.01 of formic acid regulator solution) in, at 55 DEG C, ultrasonic alkali cleaning oil removing 10min, again through ultrasonic washing 1min, then first tap water, then deionization is washed, and obtains alkali cleaning Sintered NdFeB magnet;
(3) ultrasonic activation: glacial acetic acid solution step (2) gained alkali cleaning Sintered NdFeB magnet being placed in 100mL/L, at room temperature, ultrasonic activation 40s, obtains activated sintering neodymium iron boron magnetic body;
(4) ultrasonic chemistry: step (3) gained activated sintering neodymium iron boron magnetic body is placed in described Sintered NdFeB magnet Acid electroless nickel-phosphorus plating solution, at 80 DEG C, ultrasonic plating 180min, washing, dries up.
In step (1) ~ (4), the frequency of described supersound process is 45kHz, and power is 250W.
The present embodiment gained nickel-phosphorus alloy coating thickness is 24 μm, and thickness is even, and porosity is 1.5/cm
2, magnetic loss rate is 0%; This nickel-phosphorus alloy coating evenly, be silvery white in color metal color, and by observation by light microscope, coating is without foaming and the defect such as to peel off, coating light, bath stability; Carry out bonding force test according to the thermal shock test specified in standard GB/T5270-2005 (temperature is 300 DEG C, insulation 1h), coating is without peeling, obscission, and coating is combined with matrix well; Under the neutral salt spray condition specified according to standard GB/T10125-1997 " artificial atmosphere corrosion test-salt-fog test ", (5wt%NaCl, 35 ± 1 DEG C) are tested, and the magnet resistance to neutral salt spray time reaches 300h.
From embodiment 1 ~ 3, utilize Sintered NdFeB magnet Acid electroless nickel-phosphorus plating solution gained nickel-phosphorus coating thickness of the present invention even, porosity is low, nonmagnetic rate of loss, sticking power is good, has good corrosion resistance nature, and Ni-P-plating technique flow process is simple, be easy to control.
Claims (10)
1. a Sintered NdFeB magnet Acid electroless nickel-phosphorus plating solution, is characterized in that, the pH value of described nickel plating phosphorus solution is 4.5 ~ 5.0, and it consists of:
Soluble nickel salt 25 ~ 28g/L,
Reductive agent 18 ~ 28g/L,
Compound complex agent 38 ~ 50g/L,
Buffer reagent 20 ~ 32g/L,
Promotor 0.5 ~ 1.5g/L,
Stablizer 1 ~ 3mg/L.
2. Sintered NdFeB magnet Acid electroless nickel-phosphorus plating solution according to claim 1, it is characterized in that, the compound method of described nickel plating phosphorus solution is: according to the mass ratio of solute in nickel plating phosphorus solution, respectively compound complex agent is added water together with buffer reagent and heating for dissolving, soluble nickel salt is dissolved in water, then these two kinds of solution are mixed and stir, be denoted as solution A, again reductive agent is dissolved in water, then slowly pour into while stirring in solution A, stir, be denoted as solution B, promotor and stablizer are dissolved in water, slowly pour in solution B, in the process of constant volume, use ammoniacal liquor adjust ph, .
3. Sintered NdFeB magnet Acid electroless nickel-phosphorus plating solution according to claim 1 or 2, is characterized in that, described soluble nickel salt is single nickel salt; Described reductive agent is inferior sodium phosphate; Described compound complex agent is one or more in tartrate, succinic acid or lactic acid; Described buffer reagent is sodium acetate; Described promotor is Sodium Fluoride; Described stablizer is thiocarbamide or Potassium Iodate.
4. the Acid electroless nickel-phosphorus plating technique of nickel plating phosphorus solution as described in one of claims 1 to 3, is characterized in that, comprise the following steps:
(1) ultrasonic pickling: Sintered NdFeB magnet is placed in pickle solution, at room temperature, ultrasonic pickling 20 ~ 40s, then through ultrasonic washing, conventional water wash, obtains pickling Sintered NdFeB magnet;
(2) ultrasonic alkali cleaning oil removing: step (1) gained pickling Sintered NdFeB magnet is placed in alkaline wash, at 55 ~ 60 DEG C, ultrasonic alkali cleaning oil removing 5 ~ 12min, then through ultrasonic washing, conventional water wash, obtains alkali cleaning Sintered NdFeB magnet;
(3) ultrasonic activation: step (2) gained alkali cleaning Sintered NdFeB magnet is placed in activation solution, at room temperature, ultrasonic activation 20 ~ 40s, obtains activated sintering neodymium iron boron magnetic body;
(4) ultrasonic chemistry: step (3) gained activated sintering neodymium iron boron magnetic body is placed in described Sintered NdFeB magnet Acid electroless nickel-phosphorus plating solution, ultrasonic plating 60 ~ 180min, washing, dries up.
5. Acid electroless nickel-phosphorus plating technique according to claim 4, it is characterized in that: in step (4), the temperature of described ultrasonic plating is 80 ~ 90 DEG C.
6. Acid electroless nickel-phosphorus plating technique according to claim 4 or 5, is characterized in that: in step (1), consisting of of described pickle solution: nitric acid 30 ~ 50mL/L, thiocarbamide 0.5 ~ 0.8g/L.
7. according to the described Acid electroless nickel-phosphorus plating technique of one of claim 4 ~ 6, it is characterized in that: in step (2), consisting of of described alkaline wash: sodium hydroxide 8 ~ 10g/L, 12 hypophosphite monohydrate trisodium 60 ~ 80g/L, sodium carbonate 40 ~ 60g/L, and with pH value to 9 ~ 10 of formic acid regulator solution.
8. according to the described Acid electroless nickel-phosphorus plating technique of one of claim 4 ~ 7, it is characterized in that: in step (1), (2), the time of described ultrasonic washing is 1 ~ 3min.
9. according to the described Acid electroless nickel-phosphorus plating technique of one of claim 4 ~ 8, it is characterized in that: in step (3), described activation solution is the glacial acetic acid solution of 100 ~ 200mL/L.
10. according to the described Acid electroless nickel-phosphorus plating technique of one of claim 4 ~ 9, it is characterized in that: in step (1) ~ (4), the frequency of described supersound process is 35 ~ 45kHz, and power is 100 ~ 250W.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109423670A (en) * | 2017-08-21 | 2019-03-05 | 珠海市椿田机械科技有限公司 | The preparation method and its electroplate liquid of track copper bar plating nickel on surface tungsten phosphorus alloy |
| CN112281144A (en) * | 2020-10-26 | 2021-01-29 | 中国电子科技集团公司第四十三研究所 | Ultrasonic plating method |
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