CN103556136A - Graphene-nickel-phosphorus chemical plating liquid, and preparation method and application thereof - Google Patents
Graphene-nickel-phosphorus chemical plating liquid, and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a graphene-nickel-phosphorus chemical plating liquid, and a preparation method and an application thereof. Each liter of the graphene-nickel-phosphorus chemical plating liquid comprises 0.25-1g of graphene, 20-25g of nickel sulfate, 15-20g of sodium hypophosphate, 15g of sodium acetate, 8-10g of citric acid, 4ml of lactic acid, 4ml of propionic acid, 41mg of a composite stabilizer, and the balance distilled water; and the composite stabilizer is composed of thiourea, potassium iodate and potassium iodide, and a mass ratio of thiourea to potassium iodate to potassium iodide is 1:20:20. The preparation method of the chemical plating liquid comprises the following steps: sequentially adding graphene, nickel sulfate, sodium hypophosphate, sodium acetate, citric acid, lactic acid, propionic acid and the composite stabilizer into distilled water for dissolving, and adjusting the pH value of the obtained solution to 4.2-5.6 to obtain the graphene-nickel-phosphorus chemical plating liquid. The graphene-nickel-phosphorus chemical plating liquid can be used for plating the surface of a steel alloy workpiece to form a nickel-phosphorus-graphene chemical composite coating having a good wear resistance and a high hardness.
Description
Technical field
The present invention relates to a kind of Graphene nickel-phosphorus electroless plating solution and its preparation method and application, on the surface of steel and alloy, form Graphene nickel phosphorus Composite Coatings coating.
Background technology
Electroless plating is reinforcement material preservative property, wear resistance, extends a kind of the most economic means in materials'use life-span.Ni-P is a kind of process of surface treatment developing in original single electroless plating, and has the over-all properties of matrix metal and composite particles two class materials concurrently.Research shows, the composite particles adding is conducive to change weave construction and the performance of coating, and different particle type has different effects to coating.Researchist develops the composite deposite of different particles in succession, as graphite, diamond, Al
2o
3deng.But the cladding wearability obtaining is before this generally not high, its polishing scratch sectional area is at 50-60um
2in scope.
Graphene is with its unique two-dirnentional structure and excellent electricity, optics, warm blood and mechanical property, and the extremely concern energetically of scientific research institution has become the hot research problem in the fields such as chemistry, physics.Theoretical and experimental study shows in a large number, and Graphene and derivative thereof have potential significant application value in fields such as nano-device, semiconductor material, biosensor, information storage, solar cell and hydrogen storage materials.
Yet, at present not yet relevant for the research of the chemical plating fluid that contains Graphene.
Graphene is joined to the report of making composite deposite in chemical plating fluid, as Hu Qinghua adopts chemical nickel plating method, take graphene oxide thin slice as matrix, in nickel sulfate solution, prepared Ni-Graphene, it is characterized to rear discovery, and to be deposited on the massfraction of graphene film surface Ni very high, and the dispersiveness with height, but this method does not extend to Ni Graphene is deposited on body material jointly.
Summary of the invention
One of object of the present invention is fail jointly to deposit to the technical problem of body material and a kind of Graphene nickel-phosphorus electroless plating solution is provided in order to solve above-mentioned Ni-Graphene.
The preparation method of a kind of Graphene nickel-phosphorus electroless plating solution that two of object of the present invention is to provide above-mentioned.
Three of object of the present invention is that the surface that above-mentioned Graphene nickel-phosphorus electroless plating solution is applied to steel and alloy is to form Graphene nickel phosphorus Composite Coatings coating, and the Graphene nickel phosphorus Composite Coatings coating of final gained has very strong wear resistance.
Technical scheme of the present invention
A nickel-phosphorus electroless plating solution, calculates by every liter of Graphene nickel-phosphor bath, and its composition and content are as follows:
Graphene 0.25-1g
Single nickel salt 20-25g
Inferior sodium phosphate 15-20g
Sodium acetate 15g
Citric acid 8-10g
Lactic acid 4ml
Propionic acid 4ml
One package stabilizer 41mg
Surplus is distilled water;
Described one package stabilizer, is comprised of thiocarbamide, Potassium Iodate and potassiumiodide, calculates in mass ratio, i.e. thiocarbamide: Potassium Iodate: potassiumiodide is 1:20:20.
The method preparation as follows of above-mentioned a kind of Graphene nickel-phosphor bath:
Graphene, single nickel salt, inferior sodium phosphate, sodium acetate, citric acid, lactic acid, propionic acid and one package stabilizer are added in distilled water and dissolved successively, then the sodium hydroxide solution that is 10% by concentration regulates pH value to 4.2-5.6, obtains Graphene nickel-phosphorus electroless plating solution.
Above-mentioned Graphene nickel-phosphorus electroless plating solution is applied to the surface of steel and alloy to form the method for Graphene nickel phosphorus Composite Coatings coating, specifically comprises the steps:
(1), the surperficial pre-treatment of steel and alloy workpiece
By the surface of steel and alloy workpiece, successively through 320# and the scrubbing of 280# coated abrasive working, then, by temperature, be the aqueous sodium hydroxide washes 15-20min that 80-100 ℃, mass percent concentration are 27%, use distilled water flushing 2min;
Then, then the chlorohydric acid pickling 30s that is 10% with mass percent concentration, distilled water flushing 2min used;
Finally, the hydrochloric acid activation 30s that is 5% with mass percent concentration, uses distilled water flushing 2min;
(2), step (1) steel and alloy workpiece after pretreatment is put into Graphene nickel-phosphor bath, pass into after pneumatic blending 30-60min, take out, after cleaning with distilled water, control temperature and be 15-25 ℃ be dried after, obtain the steel and alloy workpiece that surface is coated with Graphene nickel phosphorus Composite Coatings coating.
The surface of above-mentioned gained is coated with the Graphene nickel phosphorus Composite Coatings coating on the steel and alloy workpiece of Graphene nickel phosphorus Composite Coatings coating, in the mode of chemical nickel plating, Graphene particulate is jointly deposited in coating and forms Graphene nickel phosphorus Composite Coatings coating with nickel-phosphorus alloy, and the structure of formed Graphene nickel phosphorus Composite Coatings coating is born of the same parents' shape, non-crystal structure.
Beneficial effect of the present invention
A kind of Graphene nickel-phosphorus electroless plating solution of the present invention, owing to having adopted Graphene to join in chemical plating fluid as composite particles, is therefore having aspect matrix wear resistance than adding other particle better properties.
A kind of Graphene nickel-phosphorus electroless plating solution of the present invention, owing to having added the Graphene of extreme hardness in original ni-p electroless plating, therefore apply this Graphene nickel-phosphorus electroless plating solution when the plating of steel and alloy workpiece surface, the wear resistance of final formed Graphene nickel phosphorus Composite Coatings coating strengthens, and has solved the problem that nickel-phosphorus chemical plating wears no resistance.By the resistance to abrasion of Graphene, stop the friction of outer bound pair Graphene nickel phosphorus Composite Coatings coating, strengthen the wear resistance of Graphene nickel phosphorus Composite Coatings coating.
Utilize after a kind of Graphene nickel-phosphorus electroless plating solution of the present invention plating, the Graphene nickel phosphorus Composite Coatings coating of gained is the compound coating of acid high-temperature wearable, its exhibits hardness is better than simple ni-p electroless plating, and the physicals of body material is had no effect; This Graphene nickel phosphorus Composite Coatings coating is the nickel-phosphorus alloy that contains Graphene, and therefore, final formed Graphene nickel phosphorus Composite Coatings coating has very good corrosion resistance nature equally.
Accompanying drawing explanation
The surface of Fig. 1, Application Example 1 gained is coated with the scanning electron microscope (SEM) photograph of coating surface of the steel and alloy plating piece A of Graphene nickel phosphorus Composite Coatings coating;
The surface of Fig. 2, Application Example 2 gained is coated with the scanning electron microscope (SEM) photograph of coating surface of the steel and alloy plating piece B of Graphene nickel phosphorus Composite Coatings coating;
The surface of Fig. 3, Application Example 3 gained is coated with the scanning electron microscope (SEM) photograph of coating surface of the steel and alloy plating piece C of Graphene nickel phosphorus Composite Coatings coating;
The surface of Fig. 4, Application Example 4 gained is coated with the scanning electron microscope (SEM) photograph of coating surface of the steel and alloy plating piece D of Graphene nickel phosphorus Composite Coatings coating.
Embodiment
Below in conjunction with specific embodiment, technical scheme of the present invention is further described, but the present invention is not limited to following embodiment.
Various raw materials used in various embodiments of the present invention, if no special instructions, are commercially available.
embodiment 1
A nickel-phosphorus electroless plating solution, calculates by every liter of Graphene nickel-phosphor bath, and its composition and content are as follows:
Graphene 0.25g
Single nickel salt 20g
Inferior sodium phosphate 15g
Sodium acetate 15g
Citric acid 9g
Lactic acid 4ml
Propionic acid 4ml
One package stabilizer 41mg
Surplus is distilled water;
Described one package stabilizer, is comprised of thiocarbamide, Potassium Iodate and potassiumiodide, calculates in mass ratio, i.e. thiocarbamide: Potassium Iodate: potassiumiodide is 1:20:20;
The method preparation as follows of above-mentioned a kind of Graphene nickel-phosphor bath:
Graphene, single nickel salt, inferior sodium phosphate, sodium acetate, citric acid, lactic acid, propionic acid and one package stabilizer are added in distilled water and dissolved successively, and the sodium hydroxide solution that is then 10% by concentration regulates pH value to 4.2, obtains Graphene nickel-phosphorus electroless plating solution.
application Example 1
The Graphene nickel-phosphorus electroless plating solution of embodiment 1 gained is applied to the surface of steel and alloy to form Graphene nickel phosphorus Composite Coatings coating, specifically comprises the steps:
(1), steel and alloy workpiece surface pre-treatment
First, steel and alloy workpiece surface successively after 320# and the scrubbing of 280# coated abrasive working, is washed to 15-20min in the aqueous sodium hydroxide solution that is 27% successively with 80-100 ℃, mass percent concentration, use distilled water flushing 2min;
Then, the aqueous hydrochloric acid that is 10% with mass percent concentration successively washing 30s, uses distilled water flushing 2min;
Finally, the aqueous hydrochloric acid that is 5% with mass percent concentration successively washing 30s, uses distilled water flushing 2min;
(2), the good steel and alloy workpiece of step (1) surface preparation is put into the Graphene nickel-phosphorus electroless plating solution of embodiment 1 gained, under air conditions, stir after 30-60min, take out, after cleaning with distilled water, control temperature and be 15-25 ℃ be dried after, obtain the surperficial steel and alloy plating piece A that is coated with Graphene nickel phosphorus Composite Coatings coating.
The surface of above-mentioned gained is coated with the coating surface of the steel and alloy plating piece A of Graphene nickel phosphorus Composite Coatings coating, the figure that scans gained by scanning electron microscope is as shown in 1, as can be seen from Figure 1 the plating of graphene uniform, on the surface of steel and alloy matrix, is born of the same parents' shape, non-crystal structure.
The steel and alloy plating piece A that the surface of above-mentioned gained is coated with Graphene nickel phosphorus Composite Coatings coating adopts the method (Ni-P-diamond chemistry composite deposite Study on Wear-resistance) that contrasts polishing scratch sectional area, MMD-1 multifunction friction wear trier detects, and its polishing scratch sectional area is at 20-30/um
2, show that thus the Graphene nickel phosphorus Composite Coatings coating of gained has very strong wear resistance.
embodiment 2
A nickel-phosphorus electroless plating solution, calculates by every liter of Graphene nickel-phosphor bath, and its composition and content are as follows:
Graphene 1g
Single nickel salt 25g
Inferior sodium phosphate 20g
Sodium acetate 15g
Citric acid 10g
Lactic acid 4ml
Propionic acid 4ml
One package stabilizer 41mg
Surplus is distilled water;
Described one package stabilizer, is comprised of thiocarbamide, Potassium Iodate and potassiumiodide, calculates in mass ratio, i.e. thiocarbamide: Potassium Iodate: potassiumiodide is 1:20:20;
The method preparation as follows of above-mentioned a kind of Graphene nickel-phosphor bath:
Graphene, single nickel salt, inferior sodium phosphate, sodium acetate, citric acid, lactic acid, propionic acid and one package stabilizer are added in distilled water and dissolved successively, then with the sodium hydroxide solution of concentration 10%, regulate pH value to 5.6, obtain Graphene nickel-phosphorus electroless plating solution.
application Example 2
The Graphene nickel-phosphorus electroless plating solution of embodiment 2 gained is applied to the surface of steel and alloy to form Graphene nickel phosphorus Composite Coatings coating, concrete steps, with Application Example 1, finally obtain the steel and alloy plating piece B that surface is coated with Graphene nickel phosphorus Composite Coatings coating.
The surface of above-mentioned gained is coated with the coating surface of the steel and alloy plating piece B of Graphene nickel phosphorus Composite Coatings coating, the figure that scans gained by scanning electron microscope as shown in Figure 2, as can be seen from Figure 2 the plating of graphene uniform, on the surface of steel and alloy matrix, is born of the same parents' shape, non-crystal structure.
The steel and alloy plating piece B that the surface of above-mentioned gained is coated with Graphene nickel phosphorus Composite Coatings coating adopts the method for contrast polishing scratch sectional area to detect, and its polishing scratch sectional area is at 20-30/um
2, show that thus the Graphene nickel phosphorus Composite Coatings coating of gained has very strong wear resistance.
embodiment 3
A nickel-phosphorus electroless plating solution, calculates by every liter of Graphene nickel-phosphor bath, and its composition and content are as follows:
Graphene 0.75g
Single nickel salt 25g
Inferior sodium phosphate 15g
Sodium acetate 15g
Citric acid 10g
Lactic acid 4ml
Propionic acid 4ml
One package stabilizer 41mg
Surplus is distilled water;
Described one package stabilizer, is comprised of thiocarbamide, Potassium Iodate and potassiumiodide, calculates in mass ratio, i.e. thiocarbamide: Potassium Iodate: potassiumiodide is 1:20:20;
The method preparation as follows of above-mentioned a kind of Graphene nickel-phosphor bath:
Graphene, single nickel salt, inferior sodium phosphate, sodium acetate, citric acid, lactic acid, propionic acid and one package stabilizer are added in distilled water and dissolved successively, then with the sodium hydroxide solution of concentration 10%, regulate pH value to 4.8, obtain Graphene nickel-phosphorus electroless plating solution.
application Example 3
The Graphene nickel-phosphorus electroless plating solution of embodiment 3 gained is applied to the surface of steel and alloy to form Graphene nickel phosphorus Composite Coatings coating, concrete steps, with Application Example 1, finally obtain the steel and alloy plating piece C that surface is coated with Graphene nickel phosphorus Composite Coatings coating.
The surface of above-mentioned gained is coated with the coating surface of the steel and alloy plating piece C of Graphene nickel phosphorus Composite Coatings coating, the figure that scans gained by scanning electron microscope as shown in Figure 3, as can be seen from Figure 3 the plating of graphene uniform, on the surface of steel and alloy matrix, is born of the same parents' shape, non-crystal structure.
The steel and alloy plating piece C that the surface of above-mentioned gained is coated with Graphene nickel phosphorus Composite Coatings coating adopts the method for contrast polishing scratch sectional area to detect, and its polishing scratch sectional area is at 20-30/um
2, show that thus the Graphene nickel phosphorus Composite Coatings coating of gained has very strong wear resistance.
embodiment 4
A nickel-phosphorus electroless plating solution, calculates by every liter of Graphene nickel-phosphor bath, and its composition and content are as follows:
Graphene 0.75g
Single nickel salt 20g
Inferior sodium phosphate 15g
Sodium acetate 15g
Citric acid 8g
Lactic acid 4ml
Propionic acid 4ml
One package stabilizer 41mg
Surplus is distilled water;
Described one package stabilizer, is comprised of thiocarbamide, Potassium Iodate and potassiumiodide, calculates in mass ratio, i.e. thiocarbamide: Potassium Iodate: potassiumiodide is 1:20:20.
The method preparation as follows of above-mentioned a kind of Graphene nickel-phosphor bath:
Graphene, single nickel salt, inferior sodium phosphate, sodium acetate, citric acid, lactic acid, propionic acid and one package stabilizer are added in distilled water and dissolved successively, then with the sodium hydroxide solution of concentration 10%, regulate pH value to 4.8, obtain Graphene nickel-phosphorus electroless plating solution.
application Example 4
The Graphene nickel-phosphorus electroless plating solution of embodiment 4 gained is applied to the surface of steel and alloy to form Graphene nickel phosphorus Composite Coatings coating, concrete steps, with Application Example 1, finally obtain the steel and alloy plating piece D that surface is coated with Graphene nickel phosphorus Composite Coatings coating.
The surface of above-mentioned gained is coated with the coating surface of the steel and alloy plating piece D of Graphene nickel phosphorus Composite Coatings coating, the figure that scans gained by scanning electron microscope as shown in Figure 4, as can be seen from Figure 4 graphene uniform plating, on the surface of steel and alloy matrix, is born of the same parents' shape, non-crystal structure.
The steel and alloy plating piece D that the surface of above-mentioned gained is coated with Graphene nickel phosphorus Composite Coatings coating adopts the method for contrast polishing scratch sectional area to detect, and its polishing scratch sectional area is at 20-30/um
2, show that thus the Graphene nickel phosphorus Composite Coatings coating of gained has very strong wear resistance.
In sum, apply a kind of Graphene nickel-phosphorus electroless plating solution of the present invention in the surface of steel and alloy, finally form in Graphene nickel phosphorus Composite Coatings coating, the plating of graphene uniform is on the surface of steel and alloy matrix, for born of the same parents' shape, non-crystal structure, there is very strong wear resistance.
Foregoing is only the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (3)
1. a Graphene nickel-phosphor bath, is characterized in that calculating by every liter of Graphene nickel-phosphor bath, and its composition and content are as follows:
Graphene 0.25-1g
Single nickel salt 20-25g
Inferior sodium phosphate 15-20g
Sodium acetate 15g
Citric acid 8-10g
Lactic acid 4ml
Propionic acid 4ml
One package stabilizer 41mg
Surplus is distilled water;
Described one package stabilizer, is comprised of thiocarbamide, Potassium Iodate and potassiumiodide, calculates in mass ratio, i.e. thiocarbamide: Potassium Iodate: potassiumiodide is 1:20:20;
The method preparation as follows of above-mentioned a kind of Graphene nickel-phosphor bath:
Graphene, single nickel salt, inferior sodium phosphate, sodium acetate, citric acid, lactic acid, propionic acid and one package stabilizer are added in distilled water and dissolved successively, then the sodium hydroxide solution that is 10% by concentration regulates pH value to 4.2-5.6, obtains Graphene nickel-phosphorus electroless plating solution.
2. a kind of Graphene nickel-phosphor bath as claimed in claim 1 forms Graphene nickel phosphorus Composite Coatings coating for the surface at steel and alloy.
3. the method for Graphene nickel phosphorus Composite Coatings coating that forms on the surface of steel and alloy with Graphene nickel-phosphor bath as claimed in claim 2, is characterized in that comprising the steps:
(1), the surperficial pre-treatment of steel and alloy workpiece
By the surface of steel and alloy workpiece, successively through 320# and the scrubbing of 280# coated abrasive working, then, by temperature, be the aqueous sodium hydroxide washes 15-20min that 80-100 ℃, mass percent concentration are 27%, use distilled water flushing 2min;
Then, then the chlorohydric acid pickling 30s that is 10% with mass percent concentration, distilled water flushing 2min used;
Finally, the hydrochloric acid activation 30s that is 5% with mass percent concentration, uses distilled water flushing 2min;
(2), step (1) steel and alloy workpiece after pretreatment is put into Graphene nickel-phosphor bath, pass into after air 30-60min, take out, after controlling 15-25 ℃ of temperature after cleaning with distilled water and being dried, obtain the steel and alloy workpiece that surface is coated with Graphene nickel phosphorus Composite Coatings coating.
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