CN103556136B - A kind of Graphene nickel-phosphorus electroless plating solution and its preparation method and application - Google Patents
A kind of Graphene nickel-phosphorus electroless plating solution and its preparation method and application Download PDFInfo
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Abstract
The invention discloses a kind of Graphene nickel-phosphor bath and its preparation method and application, described Graphene nickel-phosphor bath, by often liter of calculating, is made up of the distilled water of 0.25-1g Graphene, 20-25g single nickel salt, 15-20g inferior sodium phosphate, 15g sodium acetate, 8-10g citric acid, 4ml lactic acid, 4ml propionic acid, 41mg one package stabilizer and surplus; Described one package stabilizer, is made up of thiocarbamide, Potassium Iodate and potassiumiodide, calculates in mass ratio, be i.e. thiocarbamide: Potassium Iodate: potassiumiodide is 1:20:20.Its preparation method adds in distilled water successively by Graphene, single nickel salt, inferior sodium phosphate, sodium acetate, citric acid, lactic acid, propionic acid and one package stabilizer and dissolves, and then adjust ph 4.2-5.6, obtains Graphene nickel-phosphorus electroless plating solution.This Graphene nickel-phosphor bath is used for carrying out on the surface of the workpiece of steel and alloy plating, and namely to form wear resistance good, the nickel phosphorus Graphene Composite Coatings coating that hardness is high.
Description
Technical field
The present invention relates to a kind of Graphene nickel-phosphorus electroless plating solution and its preparation method and application, namely form Graphene nickel phosphorus Composite Coatings coating on the surface of steel and alloy.
Background technology
Electroless plating is reinforcement material preservative property, wear resistance, extends a kind of means the most economic in materials'use life-span.Ni-P is a kind of process of surface treatment developed in original single electroless plating, and has the over-all properties of matrix metal and composite particles two class material concurrently.Research shows, the composite particles added is conducive to the weave construction and the performance that change coating, and different particle type has different effects to coating.Researchist develops the composite deposite of different particle in succession, as graphite, diamond, Al
2o
3deng.But the cladding wearability obtained before this is general not high, and its polishing scratch sectional area is at 50-60um
2in scope.
Graphene is that extremely the concern energetically of scientific research institution, has become the hot research problem in the fields such as chemistry, physics with the two-dirnentional structure of its uniqueness and excellent electricity, optics, warm blood and mechanical property.A large amount of theory and experimental study show, 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.
But, not yet there is the research about the chemical plating fluid containing Graphene at present.
Graphene is joined in chemical plating fluid the report of making composite deposite, as Hu Qinghua adopts chemical nickel plating method, with graphene oxide thin slice for matrix, Ni-Graphene has been prepared in nickel sulfate solution, to its characterize rear discovery be deposited on graphene film surface Ni massfraction very high, and there is the dispersiveness of height, but this method does not extend to and is jointly deposited on body material by Ni Graphene.
Summary of the invention
An object of the present invention is fail jointly to deposit to the technical problem of body material to solve above-mentioned Ni-Graphene and provide a kind of Graphene nickel-phosphorus electroless plating solution.
Two of object of the present invention is to provide the preparation method of above-mentioned a kind of Graphene nickel-phosphorus electroless plating solution.
Three of object of the present invention is that the surface above-mentioned Graphene nickel-phosphorus electroless plating solution being 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 kind of Graphene nickel-phosphorus electroless plating solution, calculates by often liter of Graphene nickel-phosphor bath, its composition and content 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 made up of thiocarbamide, Potassium Iodate and potassiumiodide, calculates in mass ratio, be 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 successively and dissolves, then with concentration be the sodium hydroxide solution adjust ph of 10% to 4.2-5.6, obtain 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 pre-treatment on the surface of steel and alloy workpiece
By the surface of steel and alloy workpiece successively through the scrubbing of 320# and 280# coated abrasive working, then, with temperature be 80-100 DEG C, mass percent concentration be 27% aqueous sodium hydroxide solution wash 15-20min, use distilled water flushing 2min;
Then, then be the chlorohydric acid pickling 30s of 10% with mass percent concentration, use distilled water flushing 2min;
Finally, be the hydrochloric acid activation 30s of 5% with mass percent concentration, use distilled water flushing 2min;
(2), steel and alloy workpiece after pretreatment for step (1) is put into Graphene nickel-phosphor bath, after passing into pneumatic blending 30-60min, take out, with distilled water carry out clean after control temperature be 15-25 DEG C carry out drying after, namely 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, namely in the mode of chemical nickel plating, jointly deposited in coating with nickel-phosphorus alloy by Graphene particulate and form Graphene nickel phosphorus Composite Coatings coating, the structure of the Graphene nickel phosphorus Composite Coatings coating formed 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, joins in chemical plating fluid owing to have employed Graphene as composite particles, has therefore had than adding other particle better properties in matrix wear resistance.
A kind of Graphene nickel-phosphorus electroless plating solution of the present invention, owing to adding the Graphene of extreme hardness in original ni-p electroless plating, therefore this Graphene nickel-phosphorus electroless plating solution is applied when the plating of steel and alloy workpiece surface, the wear resistance of the final Graphene nickel phosphorus Composite Coatings coating formed strengthens, and solves the problem that nickel-phosphorus chemical plating wears no resistance.Namely 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.
After utilizing 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 wear-resisting compound coating of acidic high-temperature, its exhibits hardness is better than simple ni-p electroless plating, and has no effect to the physicals of body material; This Graphene nickel phosphorus Composite Coatings coating is the nickel-phosphorus alloy containing 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 the 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 the 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 the 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 the 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 kind of Graphene nickel-phosphorus electroless plating solution, calculates by often liter of Graphene nickel-phosphor bath, its composition and content 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 made up of thiocarbamide, Potassium Iodate and potassiumiodide, calculates in mass ratio, be 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 successively and dissolves, be then the sodium hydroxide solution adjust ph to 4.2 of 10% by concentration, obtain Graphene nickel-phosphorus electroless plating solution.
application Example 1
The surface Graphene nickel-phosphorus electroless plating solution of embodiment 1 gained being applied to steel and alloy, to form Graphene nickel phosphorus Composite Coatings coating, specifically comprises the steps:
(1), steel and alloy workpiece surface pre-treatment
First, by steel and alloy workpiece surface successively after the scrubbing of 320# and 280# coated abrasive working, successively with 80-100 DEG C, mass percent concentration is wash 15-20min in the aqueous sodium hydroxide solution of 27%, uses distilled water flushing 2min;
Then, be the aqueous hydrochloric acid washing 30s of 10% successively with mass percent concentration, use distilled water flushing 2min;
Finally, be the aqueous hydrochloric acid washing 30s of 5% successively with mass percent concentration, use distilled water flushing 2min;
(2), steel and alloy workpiece good for step (1) surface preparation is put into the Graphene nickel-phosphorus electroless plating solution of embodiment 1 gained, after stirring 30-60min under air conditions, take out, with distilled water clean after control temperature be 15-25 DEG C carry out drying after, obtain the surperficial steel and alloy plating piece A being 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 of scanning gained is carried out as indicated with 1 by scanning electron microscope, as can be seen from Figure 1 the plating of graphene uniform is on the surface of steel and alloy matrix, is born of the same parents' shape, non-crystal structure.
The surface of above-mentioned gained is coated with the method (Ni-P-diamond chemical composite plating Study on Wear-resistance) of the steel and alloy plating piece A employing contrast polishing scratch sectional area of Graphene nickel phosphorus Composite Coatings coating, MMD-1 multifunction friction wear trier detects, and its polishing scratch sectional area is at 20-30/um
2, show that the Graphene nickel phosphorus Composite Coatings coating of gained has very strong wear resistance thus.
embodiment 2
A kind of Graphene nickel-phosphorus electroless plating solution, calculates by often liter of Graphene nickel-phosphor bath, its composition and content 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 made up of thiocarbamide, Potassium Iodate and potassiumiodide, calculates in mass ratio, be 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 successively and dissolves, then use the sodium hydroxide solution adjust ph to 5.6 of concentration 10%, 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 of scanning gained is carried out as shown in Figure 2 by scanning electron microscope, as can be seen from Figure 2 the plating of graphene uniform is 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 the Graphene nickel phosphorus Composite Coatings coating of gained has very strong wear resistance thus.
embodiment 3
A kind of Graphene nickel-phosphorus electroless plating solution, calculates by often liter of Graphene nickel-phosphor bath, its composition and content 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 made up of thiocarbamide, Potassium Iodate and potassiumiodide, calculates in mass ratio, be 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 successively and dissolves, then use the sodium hydroxide solution adjust ph to 4.8 of concentration 10%, 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 of scanning gained is carried out as shown in Figure 3 by scanning electron microscope, as can be seen from Figure 3 the plating of graphene uniform is 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 the Graphene nickel phosphorus Composite Coatings coating of gained has very strong wear resistance thus.
embodiment 4
A kind of Graphene nickel-phosphorus electroless plating solution, calculates by often liter of Graphene nickel-phosphor bath, its composition and content 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 made up of thiocarbamide, Potassium Iodate and potassiumiodide, calculates in mass ratio, be 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 successively and dissolves, then use the sodium hydroxide solution adjust ph to 4.8 of concentration 10%, 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 of scanning gained is carried out as shown in Figure 4 by scanning electron microscope, as can be seen from Figure 4 graphene uniform plating is 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 the Graphene nickel phosphorus Composite Coatings coating of gained has very strong wear resistance thus.
In sum, apply a kind of Graphene nickel-phosphorus electroless plating solution of the present invention in the surface of steel and alloy, in final formation 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 be only the present invention conceive under basic explanation, and according to any equivalent transformation that technical scheme of the present invention is done, all should protection scope of the present invention be belonged to.
Claims (2)
1. a Graphene nickel-phosphor bath, is characterized in that calculating by often liter of Graphene nickel-phosphor bath, its composition and content 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 made up of thiocarbamide, Potassium Iodate and potassiumiodide, calculates in mass ratio, be 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 successively and dissolves, then with concentration be the sodium hydroxide solution adjust ph of 10% to 4.2-5.6, obtain Graphene nickel-phosphorus electroless plating solution.
2. a kind of Graphene nickel-phosphor bath as claimed in claim 1 is used for forming Graphene nickel phosphorus Composite Coatings coating on the surface of steel and alloy.
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| CN103833231B (en) * | 2014-03-06 | 2016-02-10 | 上海应用技术学院 | A kind of have glass of graphene oxide nickel-phosphorus composite deposit and preparation method thereof |
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| CN106868486B (en) * | 2015-12-14 | 2019-07-23 | 宝山钢铁股份有限公司 | A kind of agents for film forming treatment and film-forming process of compound chemical composition coating used for magnesium alloy |
| CN105821465A (en) * | 2016-05-09 | 2016-08-03 | 南昌航空大学 | Preparation method for silver and graphene composite coating of cyanide-free system |
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| CN106756905A (en) * | 2017-01-20 | 2017-05-31 | 上海应用技术大学 | Compound nickel-base plating coat of nano-graphene and preparation method thereof |
| CN108165958A (en) * | 2018-01-25 | 2018-06-15 | 广东工业大学 | A kind of method of red copper surface chemical Ni-P plating-graphene composite deposite |
| WO2019161512A1 (en) | 2018-02-26 | 2019-08-29 | Graphene Leaders Canada (Glc) Inc. | Electroless plating of objects with carbon-based material |
| CN112746197A (en) * | 2020-12-28 | 2021-05-04 | 江苏省特种设备安全监督检验研究院 | Preparation method of graphene-reinforced nickel-based nano composite powder metallurgy material |
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