CN1676674A - Method for preparing nickel-phosphor alloy base composite cladding containing nano particle - Google Patents

Abstract

This invention is about the preparing method of Ni-P alloy base composite deposited layer which contains nano SiO2 microns. The invention uses electrodeposition plating, and the electroplate liquid is made up of : NiSO4.6H2O 300g/L, NiCl2.6H2O 45g/L, H3BO3 40g/L, H3PO3 15g/L. The value of PH is 1-2, and the solution is distilled water or de-ionized water. Besides, nanometer SiO2 microboulders which have been treated should be added, and the dosis should be 10 g/L. Before the microboulders are added, in the method of pulse electrodeposition plating, the positive pole should be large square of pure Ni plate, while the negative pole is the body which will be plated with. During the process of plating, pulse electricity goes into the solution. The average electricity density is 5A/square decimeter, while the impulse width is ton = 1 ms, and the duty ratio is 1 : 7. What is more, the temperature of the electroplate liquid should be kept as 60 deg.C. At last, we can get the Ni-P alloy base composite deposited layer which contains nanometer SiO2 microns on the metal substrate material. This composite layer made in this invention has high hardness, while the layer is homogeneous and smooth, and the pattern structure is also quite satisfactory.

Description

The preparation method who contains the nickel-phosphor alloy base composite cladding of nanoparticle

Technical field

The present invention relates to a kind of nanometer SiO that contains ₂The preparation method of the nickel-phosphor alloy base composite cladding of particulate; Belong to Metal plating Technology field.

Background technology

Plating has long history as the surface treatment means, and its range of application is very wide, all need use the electroplating technology technology at many industrial circles and come process metal surfaces.Composite deposite is by the metal electrodeposition method, and a kind of or several insoluble solia particles are mingled with formed special coating in the metal plating equably.Composite plating has been considered to current solution high temperature corrosion, hot strength and wearing and tearing, and a kind of up-and-coming method of some problem such as wearing and tearing in particular cases, is a kind of advanced method of producing matrix material.

Summary of the invention

The object of the present invention is to provide a kind of nanometer SiO that contains ₂The method of the nickel-phosphor alloy base composite cladding of particulate.

Another object of the present invention is to by in the Ni-P system, adding nanometer SiO ₂Particulate with the method for pulse plating with composite electrodeposition, is prepared Ni-P-SiO under certain condition ₂Composite deposite.

A kind of preparation method who contains the nickel-phosphor alloy base composite cladding of nanoparticle of the present invention is characterized in that this method comprises following processing step:

A. be ready to desire the metal base material of coating, this material needs operations such as prior economy-combat grinding and polishing light, washing, oil removing, washing, pickling;

B. treated good metal base material is positioned in the constant temperature plating tank, electroplates, electroplate liquid is for being added with nanometer SiO ₂The nickel of particulate-phosphorus base composite electric plating bath; Consisting of of electroplate liquid: NiSO ₄6H ₂O 300g/L, NiCl ₂6H ₂O 45g/L, H ₃BO ₃40g/L, H ₃PO ₃15g/L, the pH value is 1～2, wherein solvent is deionized water or distilled water;

C. in above-mentioned electroplate liquid, add nanometer SiO ₂Powdery particulate, addition are 10g/L; Before the interpolation, nanometer SiO ₂Particulate needs process processing earlier, and treatment process is: with SiO ₂Particulate is earlier wetting and with ultrasonic dispersing 10 minutes with less water, adds the low quantity of surfactant hexadecyl trimethyl ammonium bromide again, and the usefulness ultrasonic dispersing adds in the above-mentioned electroplate liquid after 40 minutes more subsequently; And then this electroplate liquid continued ultra-sonic dispersion 1 hour;

D. adopt pulse electrodeposition coating mode, anode is a big area pure nickel plate, is negative plate with the plating piece, feeds pulsed current, and average current density is 5A/dm ², pulsewidth is t _On=1ms, dutycycle is 1: 7; The temperature of electroplate liquid remains 60 ℃; Can on metal base material, obtain containing nanometer SiO at last ₂The nickel-phosphor alloy base composite cladding of particulate.

The advantage of the inventive method is: introduce nanometer SiO in nickel-cobalt-tungsten-nickel-phosphorus alloy electroplating ₂Behind the particulate, can further improve the hardness of coating.Adopt the nickel-phosphor alloy coating that obtains under pulse and the direct current electrode position condition to compare in addition, then the hardness of the nickel of pulse plating gained-phosphorus alloy layer is higher, and the pattern of coating is also better.

Embodiment

Now the specific embodiment of the present invention is described in the back:

Embodiment one: earlier with metal base material, promptly copper sheet is through mechanical grinding polishing, washing, the ultrasonic oil removing of acetone, washing, electrochemical deoiling, washing, the weak etch of acid, washing; Be ready to treated good base material copper sheet; Treated good metal base material is positioned in the constant temperature plating tank, electroplates, electroplate liquid is for being added with nanometer SiO ₂The nickel of particulate-phosphorus base composite electric plating bath; Consisting of of electroplate liquid: NiSO ₄6H ₂O 300g/L, NiCl ₂6H ₂O 45g/L, H ₃BO ₃40g/L, H ₃PO ₃15g/L, the pH value is 1～2, wherein solvent is a distilled water; In above-mentioned electroplate liquid, add nanometer SiO ₂Powdery particulate, addition are 10g/L; Before the interpolation, nanometer SiO ₂Particulate needs process processing earlier, and treatment process is: with SiO ₂Particulate is earlier wetting and with ultrasonic dispersing 10 minutes with less water, adds the low quantity of surfactant hexadecyl trimethyl ammonium bromide again, and the usefulness ultrasonic dispersing adds in the above-mentioned electroplate liquid after 40 minutes more subsequently; And then this electroplate liquid continued ultra-sonic dispersion 1 hour; Adopt pulse electrodeposition coating mode, anode is a big area pure nickel plate, is negative plate with the plating piece, feeds pulsed current, and average current density is 5A/dm ², pulsewidth is t _On=1ms, dutycycle is 1: 7; The temperature of electroplate liquid remains 60 ℃; Can on copper sheet, obtain containing nanometer SiO at last ₂Nickel-the phosphorus of particulate and auri composite deposite.

The resulting composite deposite of present embodiment method through X-ray diffraction analysis, can obtain that crystallite is evenly distributed, good dispersion, pattern coating structure preferably.By transmission electron microscope observation, nanometer SiO in the coating ₂The median size of particulate is 6-7nm.

Claims (1)

1. a preparation method who contains the nickel-phosphor alloy base composite cladding of nanoparticle is characterized in that, this method comprises following processing step:

A. be ready to the metal base material of desire plating, this material needs operations such as prior economy-combat grinding and polishing light, washing, oil removing, washing, pickling.

B. treated good metal base material is positioned in the constant temperature plating tank, electroplates.Electroplate liquid is for being added with nanometer SiO ₂The nickel of particulate-phosphorus system plating solution; Consisting of of electroplate liquid: NiSO ₄6H ₂O 300g/L, NiCl ₂6H ₂O 45g/L, H ₃BO ₃40g/L, H ₃PO ₃15 g/L, pH value are 1～2, and wherein solvent is deionized water or distilled water.

C. in above-mentioned electroplate liquid, add nanometer SiO ₂Powdery particulate, addition are 10g/L; Before the interpolation, nanometer SiO ₂Particulate needs process processing earlier, and treatment process is: with SiO ₂Particulate is earlier wetting and with ultrasonic dispersing 10 minutes with a small amount of distilled water, adds the low quantity of surfactant hexadecyl trimethyl ammonium bromide again, and the usefulness ultrasonic dispersing adds in the above-mentioned electroplate liquid after 40 minutes more subsequently; And then this electroplate liquid continued ultra-sonic dispersion 1 hour.

D. adopt pulse electrodeposition coating mode, anode is a big area pure nickel plate, is negative plate with the plating piece, feeds pulsed current, and average current density is 5A/dm ², pulsewidth is t _On=1ms, dutycycle is 1: 7; The temperature of electroplate liquid remains 60 ℃; Can on metal base material, obtain containing nanometer SiO at last ₂The nickel-phosphor alloy base composite cladding of particulate.