CN1410592A - Method of supersonic chemical plating nickel phosphorus of powder metallurgy material - Google Patents

Method of supersonic chemical plating nickel phosphorus of powder metallurgy material Download PDF

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Publication number
CN1410592A
CN1410592A CN 01128224 CN01128224A CN1410592A CN 1410592 A CN1410592 A CN 1410592A CN 01128224 CN01128224 CN 01128224 CN 01128224 A CN01128224 A CN 01128224A CN 1410592 A CN1410592 A CN 1410592A
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plating
ultrasonic
oil removing
agent
follows
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CN1150349C (en
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吴杰
金花子
吴敏杰
崔新宇
熊天英
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Institute of Metal Research of CAS
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Institute of Metal Research of CAS
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Abstract

In the invention, the sodium hypopphosphite is as the reducing agent of the bath, nickel sulfate as the main salt, with the complexing agent, accelerating agent and stabilizing agent being added. The ultrasonic chemical plating is adopted that utilizes the mechanical energy of the ultrasonic vibration, making the bath deposit nickel and phosphor under the catalysis of the metal surface and the chemical reduction method controlled. The plating procedure includes the steps of oil removal, rust removal, activation, chemical plating and post treatment. The multiple complexing, accelerating and stabilizing agents raises the stability of the bath. The plating speed is adjustable. The even, compact nickel and phosphor plating layer covers the surface of the base body of powder metallurgical material so as to increase the service life of the material and provide wide application area.

Description

Method of supersonic chemical plating nickel phosphorus of powder metallurgy material
Technical field
The present invention relates to field of chemical processing of material, specifically method of supersonic chemical plating nickel phosphorus of powder metallurgy material.
Background technology
The application of mmaterial in recent years is very rapid with development, and this material is to be synthesized by various powders mostly, because technological reason makes material surface have many micropores.For example neodymium iron boron (NdFeB) permanent magnet material adopts the powder metallurgy process preparation, and the NdFeB permanent magnet is the SmCo that continues 5And Sm 2Co 17Third generation rare earth permanent-magnetic material afterwards, owing to having higher saturation magnetization, coercive force and magnetic energy product, it becomes critical function material in the Modern High-Tech field, but because the easy oxidation and rusting of NdFeB permanent magnet, solidity to corrosion difference and its widespread use is restricted.
In the prior art, material surface is handled close technology adopt electroless plating and electric plating method more, in electroless plating technology, neutral electroless plating, acid chemical plating and alkaline electroless plating, these chemical plating methods have developed decades, according to incompletely statistics, have at present ripe formula for chemical plating nickel more than 200 kinds (" electroless plating is theoretical and put into practice " the 6th page in the world at least, National Defense Industry Press), adopt the sonochemistry electroplating method not appear in the newspapers as yet for mmaterial.Generally adopt chemical nickel plating coating or electro-coppering nickel composite deposite as protective layer at present in the world for the Nd-Fe-B powder powder metallurgy material, the 32nd volume first phase of February calendar year 2001 " magneticsubstance and device " has been introduced the analysis of sintered Nd Fe B magnet plating defect, after electroplating processes, pit in irregular shape or hollow hole usually appear in magnets N i coating or some position of Zn coating, influence the use of quality of coating and magnet; In addition, generally adopt chemical nickel plating coating or electro-coppering nickel composite deposite as protective layer at present in the world, wherein chemical nickel plating coating porosity is big, and anticorrosion effect is poor, and electroplates problems such as there being quality of coating instability in uneven thickness.
Summary of the invention
The purpose of this invention is to provide a kind of material coating imporosity, thickness is even and solidity to corrosion is strong method of supersonic chemical plating nickel phosphorus of powder metallurgy material of making.
To achieve these goals, technical scheme of the present invention be plating bath with inferior sodium phosphate as reductive agent, single nickel salt is as main salt, additional complexing agent, accelerator, stablizer adopt ultrasonic electroless deposition technique, utilize the mechanical energy of ultrasonic oscillation, make plating bath under the katalysis of metallic surface, carry out nickel phosphorus deposition process through the control chemical reduction method, comprise oil removing, rust cleaning, activation, ultrasonic chemistry and post-processing step, specific as follows:
(1) oil removing
A. vacuum oil removing:
Adopt 120～200 ℃, 0.5～3 hour vacuum heat treatment;
B. alkali lye oil removing:
After the vacuum oil removing, carry out the alkali lye oil removing, alkali lye pH value is 8～10.5, the alkali lye prescription is as follows:
Na 2CO 3：5～20g/l；Na 3PO 4·12H 2O：10～30g/l；
Na 2SiO 3: 5～20g/l; OP-10 emulsifying agent: 1～5g/l;
Alkali liquid temperature is 60～80 ℃, adopts ultrasonic wave simultaneously, and ultrasonic frequency is that 19～80kHz, power are 50～500w, and the treatment time is 5～10 minutes;
(2) rust cleaning
Employing concentration is 5～40% HNO 3Carry out pickling, the time is 5～100 seconds;
(3) activation
Employing concentration is 1～10% H 2SO 4As activation solution, at room temperature soak time is: 5～50 seconds;
(4) ultrasonic chemistry
As reductive agent, single nickel salt is as main salt with inferior sodium phosphate for plating bath, and additional complexing agent, accelerator, stablizer adopt ultrasonic oscillation simultaneously, and the prescription of plating bath is as follows:
Main salt: single nickel salt NiSO 46H 2O:20～30g/l;
Reductive agent: inferior sodium phosphate NaH 2PO 2H 2O:20～40g/l;
Complexing agent: sodium acetate NaAC3H 2O:10～25g/l;
Propionic acid C 2H 5COOH:5～30g/l;
DL-oxysuccinic acid CHOHCH 2(COOH) 2: 5～30g/l;
Glycine NH 2CH 2COOH:1～10g/l;
EDTAC 10H 16N 2O 8：1～10g/l；
Trisodium Citrate Na 3C 6H 5O 72H 2O:5～40g/l;
Accelerator: Succinic Acid (CH 2COOH) 2: 5～30g/l;
Stablizer: lead acetate (Pb 2+): 1～5ppm; Thiocarbamide H 2NCSNH 2: 0.5～5ppm;
The ultrasonic chemistry processing parameter is as follows:
Frequency 19～80kHz, power 50～500W, pH6.5～7.5,
70～85 ℃ of temperature, plating speed is 10～60 μ m/ hours;
(5) aftertreatment
Adopt CrO 3Carry out sealing of hole and handle processing parameter:
CrO 3: 1～10g/l, temperature: 70～85 ℃, time: 10～20 minutes.
Can also carry out the secondary electroless plating as requested after the described step 4, its electroplate liquid formulation is as follows:
Main salt: single nickel salt NiSO 46H 2O:20～30g/l;
Reductive agent: inferior sodium phosphate NaH 2PO 2H 2O:20～40g/l;
Complexing agent: sodium acetate NaAC3H 2O:20～25g/l;
DL-oxysuccinic acid CHOHCH 2(COOH) 2: 5～25g/l;
Glycine NH 2CH 2COOH:1～10g/l;
Trisodium Citrate Na 3C 6H 5O 72H 2O:2～10g/l;
Lactic acid CH 3CHOHCOOH:5～25g/l;
Propionic acid C 2H 5COOH:5～25g/l;
Accelerator: Succinic Acid (CH 2COOH) 2: 5～25g/l;
Stablizer: lead acetate (Pb 2+): 1～5ppm;
Thiocarbamide H 2NCSNH 2: 0.5～5ppm;
The chemical plating technology parameter is as follows:
Temperature: 86～90 ℃, pH:4.4～4.8, load ratio: 0.4～2,
Loop cycle: 5～6, plating speed: 12～16 μ m/ hours;
The principle of the invention: utilize the mechanical energy of ultrasonic oscillation to make plating bath produce many holes at the matrix table, these hole sustained oscillations produce powerful shock action to matrix surface, i.e. ultrasonic cavitation, ultrasonic cavitation can cause a large amount of activity freely to produce, make the matrix surface activation, quicken chemical reaction; Strengthen molecular impact on the other hand, make attached to the bubble in matrix surface and the hole and can in time discharge, thereby the nickel ion reduce deposition in the plating bath is had on the surface of catalytic activity, make that matrix surface plating one deck is even compact, imporous nickel-phosphorus coating, matrix is played protective effect.
Beneficial effect of the present invention is as follows:
1. coating imporosity and thickness are even, thereby have improved the corrosion resisting property of mmaterial.The ni-p electroless plating prescription of the application of the invention development, adopt ultrasonic chemistry, utilize the mechanical energy of ultrasonic oscillation to make plating bath produce many holes at matrix surface, these holes produce powerful shock action to matrix surface, make the matrix surface activation, quicken chemical reaction, thus, imporous nickel-phosphorus coating even compact at matrix surface plating one deck.
2. improve the work-ing life of mmaterial, widen it and answer the field.When the nickel-phosphorus coating thickness that adopts the present invention to form at matrix surface reaches 30～40 microns, damp and hot, the High-Voltage Experimentation life-span is more than 500 hours, the salt mist experiment life-span is more than 300 hours, thereby make the mmaterial range of application more extensive, can be applied to fields such as electronics, computer, automobile, medical treatment.
3. the present invention adopts multiple complexing agent and accelerator, stablizer, has improved bath stability, and plating speed can be regulated, and thickness of coating is even; Chemical plating method of the present invention is compared with plating, is easy to control, and electroplates owing to fringing effect, and current density is inhomogeneous, causes thickness of coating inhomogeneous.
4. the present invention can shorten the oil removing time by adopting vacuum oil removing and the oil removing of ultrasonic wave alkali lye, strengthens deoiling effect, improves processing quality.
5. to adopt concentration be 1～10% H in the present invention 2SO 4As activation solution, can remove the vaporization membrane as thin as a wafer on the specimen surface, and form uniform forming core active centre thereon, improve nickel plating phosphorus effect.
Embodiment
Be described in further detail the present invention below by embodiment.
Embodiment 1
Adopt the inventive method to carry out plating on powder metallurgy TiC cutter material surface, specific as follows:
(1) oil removing
A. vacuum oil removing
Adopt 200 ℃, 1 hour vacuum heat treatment, remove the greasy dirt on TiC cutter material top layer, because the TiC cutter material is a mmaterial, surface irregularity, hole is many, and greasy dirt is had stronger adsorptive power, therefore adopts the vacuum oil removing; In addition, also can prevent the aerial oxidation of TiC cutter;
B. alkali lye oil removing
After the vacuum oil removing, carry out the alkali lye oil removing, alkali lye pH value is 10, the alkali lye prescription is as follows:
Na 2CO 3：15g/l；Na 3PO 4·12H 2O：20g/l；
Na 2SiO 3: 5g/l; OP-10 emulsifying agent: 1g/l;
(OP-10 emulsifying agent, commercially available prod, source: reagent shop, Shenyang)
Alkali liquid temperature is 60 ℃, adopts ultrasonic wave simultaneously, and ultrasonic frequency is that 19kHz, power are 200w, and the treatment time is 5 minutes;
For guaranteeing the bonding strength of TiC cutter material overlay coating, after the vacuum oil removing, also should carry out the alkali lye oil removing, the pH value of alkaline solution is not more than 10.5; In addition, in order to improve deoiling effect, adopt ultrasonic wave simultaneously, ultrasonic wave can be strengthened the oil removing process, shortens the oil removing time, improves processing quality;
(2) rust cleaning
Employing concentration is 20% HNO 3Carry out pickling, the time is 30 seconds;
(3) activation
Employing concentration is 10% H 2SO 4As activation solution, at room temperature soak time is 15 seconds, in order to remove the vaporization membrane as thin as a wafer on the specimen surface, and the uniform forming core of shape active centre thereon, before carrying out electroless plating, carry out activation treatment;
(4) ultrasonic chemistry
As reductive agent, single nickel salt is as main salt with inferior sodium phosphate for plating bath, and additional complexing agent, accelerator, stablizer adopt ultrasonic oscillation simultaneously, and the prescription of plating bath is as follows:
Main salt: single nickel salt: 28g/l; Reductive agent: inferior sodium phosphate: 35g/l;
Complexing agent: sodium acetate: 22g/l; Propionic acid: 15g/l; DL-oxysuccinic acid: 25g/l;
Glycine: 8g/l; EDTA:6g/l; Trisodium Citrate: 30g/l;
Accelerator: Succinic Acid: 25g/l;
Stablizer: lead acetate (Pb 2+): 5ppm; Thiocarbamide H 2NCSNH 2: 5ppm;
The ultrasonic chemistry processing parameter:
Frequency: 40kHz, power: 400W, pH:7.5, temperature: 80 ℃, time: 30 minutes, the plating fast 40 μ m/ hours; Various ions violent random encounters under the effect of ultrasonic wave field under the katalysis of metallic surface, is carried out nickel phosphorus deposition through the control chemical reduction method in the plating bath, can plate evenly complete coating of one deck, and outward appearance is silvery white in color and coating is combined;
(5) aftertreatment
Adopt CrO 3Carry out sealing of hole and handle processing parameter:
CrO 3: 10g/l, temperature: 70 ℃, time: 10 minutes;
Through above-mentioned processing, obtaining thickness of coating is 20 microns.
Embodiment 2
Difference from Example 1 is:
Adopt the inventive method to carry out plating at neodymium-iron-boron permanent magnetic material surface, as reductive agent, single nickel salt is as main salt with inferior sodium phosphate for plating bath, and additional complexing agent, accelerator, stablizer adopt ultrasonic electroless deposition technique and secondary chemical plating method; At first NdFeB material is carried out chamfered, adopt mechanical barreling chamfering method, insert in the airtight ceramic roller by NdFeB material sample and 1.0: 1.0 amount of corundum sand volume ratio, total amount accounts for 3/4 of total drum volume, add alcohol submergence sample then, start cylinder, drum rotational speed is 30r/min, and the time is 36 hours;
The prescription of ultrasonic chemistry plating bath is as follows:
Main salt: NiSO 46H 2O:27g/l; Reductive agent: NaH 2PO 2H 2O:33g/l;
Complexing agent: NaAC3H 2O:12g/l; Propionic acid: 6g/l; DL-oxysuccinic acid: 8g/l;
Glycine: 2g/l; EDTA:2g/l; Trisodium Citrate: 15g/l;
Accelerator: Succinic Acid: 10g/l;
Stablizer: lead acetate (Pb 2+) 1ppm; Thiocarbamide: 1ppm;
Ultrasonic chemistry processing parameter: frequency 19kHz, power 200W, pH6.5,70 ℃ of temperature, were plated fast 40 μ m/ hours at 10 minutes time;
Secondary chemical plating bath prescription is as follows:
Main salt: NiSO 46H 2O:27g/l; Reductive agent: NaH 2PO 2H 2O:30g/l;
Complexing agent: NaAC3H 2O:20g/l; DL-oxysuccinic acid: 12g/l; Glycine: 1g/l;
Trisodium Citrate: 2g/l; Lactic acid: 10g/l; Propionic acid: 10g/l;
Accelerator: Succinic Acid: 16g/l; Stablizer: lead acetate: 2ppm; Thiocarbamide: 2ppm;
The chemical plating technology parameter is as follows:
Temperature: 86 ℃, 2 hours time, pH:4.6, loading ratio: 1, loop cycle: 5, plating speed: 12 μ m/ hours; Various ions carry out nickel phosphorus deposition process through the control chemical reduction method in the plating bath under the katalysis of metallic surface;
The aftertreatment technology parameter:
CrO 3: 3g/l, temperature: 78 ℃, time: 15 minutes;
Through above-mentioned processing, obtaining thickness of coating is 30 microns.
Relevant comparative example
Adopt the present invention to compare for the corrosion resisting property that neodymium iron boron prepares protective coating and relevant chemical plating method, as shown in table 1:
Table 1
Chemical plating method Salt mist experiment Porosity Damp and hot experiment High-Voltage Experimentation
Acidic bath: can't plating
Alkali plating solution (30 microns) 24 hours 2％ 72 hours 48 hours
Neutral plating bath (30 microns) 120 hours 1％ 240 hours 226 hours
The present invention's (30 microns) ＞300 hours Do not have ＞500 hours ＞500 hours
Found out by table 1, because neodymium iron boron is mmaterial, can't carry out plating in common acidic bath, though can plate in alkali plating solution, coating stress is big, poor adhesive force and porosity are big, and edge begins to come off when salt mist experiment.

Claims (2)

1. method of supersonic chemical plating nickel phosphorus of powder metallurgy material, it is characterized in that: be as reductive agent with inferior sodium phosphate, single nickel salt is as main salt, additional complexing agent, accelerator, stablizer adopt the sonochemistry electroplating method, utilize the mechanical energy of ultrasonic oscillation, make plating bath under the katalysis of metallic surface, carry out nickel phosphorus deposition process through the control chemical reduction method, comprise oil removing, rust cleaning, activation, ultrasonic chemistry and post-processing step, specific as follows:
1) oil removing
A. vacuum oil removing:
Adopt 120～200 ℃, 0.5～3 hour vacuum heat treatment;
B. alkali lye oil removing:
After the vacuum oil removing, carry out the alkali lye oil removing, alkali lye pH value is 8～10.5, the alkali lye prescription is as follows:
Na 2CO 3：5～20g/l；Na 3PO 4·12H 2O：10～30g/l；
Na 2SiO 3: 5～20g/l; OP-10 emulsifying agent: 1～5g/l;
Alkali liquid temperature is 60～80 ℃, adopts ultrasonic wave simultaneously, and ultrasonic frequency is that 19～80kHz, power are 50～500w, and the treatment time is 5～10 minutes;
2) rust cleaning
Employing concentration is 5～40% HNO 3Carry out pickling, the time is 5～100 seconds;
3) activation
Employing concentration is 1～10% H 2SO 4As activation solution, at room temperature soak time is: 5～50 seconds;
4) ultrasonic chemistry
As reductive agent, single nickel salt is as main salt with inferior sodium phosphate for plating bath, and additional complexing agent, accelerator, stablizer adopt ultrasonic oscillation simultaneously, and the prescription of plating bath is as follows:
Main salt: single nickel salt: 20～30g/l; Reductive agent: inferior sodium phosphate: 20～40g/l;
Complexing agent: sodium acetate: 10～25g/l; Propionic acid: 5～30g/l; DL-oxysuccinic acid: 5～30g/l;
Glycine: 1～10g/l; EDTA:1～10g/l; Trisodium Citrate: 5～40g/l;
Accelerator: Succinic Acid: 5～30g/l; Stablizer: lead acetate: 1～5ppm; Thiocarbamide: 0.5～5ppm;
The ultrasonic chemistry processing parameter is as follows:
Frequency 19～80kHz, power 50～500W, pH6.5～7.5,70～85 ℃ of temperature,
Plating speed is 10～60 μ m/ hours;
5) aftertreatment
Adopt CrO 3Carry out sealing of hole and handle processing parameter:
CrO 3: 1～10g/l, temperature: 70～85 ℃, time: 10～20 minutes.
2. according to the described method of supersonic chemical plating nickel phosphorus of powder metallurgy material of claim 1, it is characterized in that: carry out the secondary electroless plating after the described step 4, its electroplate liquid formulation is as follows:
Main salt: single nickel salt: 20～30g/l; Reductive agent: inferior sodium phosphate: 20～40g/l;
Complexing agent: sodium acetate: 20～25g/l; DL-oxysuccinic acid: 5～25g/l; Glycine: 1～10g/l;
Trisodium Citrate: 2～10g/l; Lactic acid: 5～25g/l; Propionic acid: 5～25g/l;
Accelerator: Succinic Acid: 5～25g/l; Stablizer: lead acetate: 1～5ppm; Thiocarbamide: 0.5～5ppm;
The chemical plating technology parameter is as follows:
Temperature: 86～90 ℃, pH:4.4～4.8, load ratio: 0.4～2,
Loop cycle: 5～6, plating speed: 12～16 μ m/ hours.
CNB01128224XA 2001-09-29 2001-09-29 Method of supersonic chemical plating nickel phosphorus of powder metallurgy material Expired - Fee Related CN1150349C (en)

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