CN108893730B - A kind of electroless plating pearl nickel plating solution and method - Google Patents

Abstract

A plating solution and method for chemically plating pearl nickel, which relate to a pretreatment method on a low-carbon steel sheet and a preparation method using an electroless pearl nickel plating solution. The invention solves the problems of complicated instruments, accurate operation, difficult control, poor coating uniformity and the like in the traditional pearl nickel preparation method. The method of the invention is as follows: 1. the configuration of the alkaline washing solution; 2. the configuration of the surface pre-plating solution; 3. the configuration of the electroless plating solution; → Alkaline cleaning and degreasing → Water washing → Pickling activation → Water washing → Drying → Pre-plating → Electroless plating. The pearl nickel prepared by the invention not only has a uniform coating layer, but also can reduce consumption in terms of technology, so as to achieve energy saving and emission reduction.

Description

A kind of electroless plating pearl nickel plating solution and method

technical field

The invention relates to a pearl nickel plating process and a plating solution, in particular to a plating solution and a method for chemically plating pearl nickel.

Background technique

Electroless nickel plating is a method of depositing a layer of nickel on the surface of metal parts by redox without external current. Used to improve corrosion and abrasion resistance, increase gloss and aesthetics. It is suitable for bright nickel plating of small parts with tubular or complex shape without polishing. Generally, the workpiece to be plated is immersed in a mixed solution of nickel sulfate, sodium hypophosphite, sodium acetate and boric acid, and changes at a certain acidity and temperature, and the nickel ions in the solution are reduced to atoms by sodium hypophosphite It is deposited on the surface of the workpiece to form a fine and bright nickel coating.

Pearl nickel is also known as satin nickel, sardine nickel, etc. Because of its unique surface morphology, it has a pearl-like and elegant luster visually, and it does not reflect as strongly as bright nickel, which makes people feel very comfortable. Because of this, long-term observation of pearl nickel will not cause visual fatigue, so now people will choose pearl nickel products more, and pearl nickel is favored in the fields of aerospace, life, and scientific research. Pearl nickel has a non-smooth and uneven surface, and light will be diffusely reflected on its surface. At the same time, its porosity is low, its internal stress is lower than that of normal bright nickel and dark nickel, and its corrosion resistance is very good. It can be touched by hand. Will not leave fingerprints easily. At present, many European and American countries and Japan have adopted pearl nickel as one of the anti-corrosion materials and promoted them.

SUMMARY OF THE INVENTION

The purpose of the present invention is to provide a plating solution and method for preparing pearl nickel by chemical plating, which solves the problems of monotonous preparation method of pearl nickel and uneven coating.

A kind of plating solution and method for chemical plating pearl nickel of the present invention is carried out according to the following steps:

1. Preparation of alkaline washing solution: Dissolve sodium hydroxide, sodium phosphate, sodium silicate, sodium carbonate and sodium lauryl sulfate in deionized water for use;

2. Preparation of pre-plating solution: dissolve zinc oxide, zinc dihydrogen phosphate, phosphoric acid, citric acid, sodium fluoride, sodium dodecylbenzene sulfonate, and sodium molybdate in deionized water, adjust the pH, and stand by;

3. Preparation of chemical plating solution:

(1) Acid electroless plating solution: dissolve nickel sulfate, sodium hypophosphite, citric acid, anhydrous sodium acetate, sodium chloride, emulsifier OP-10, potassium iodate, sodium dihexyl succinate sulfonate In deionized water, adjust the pH for later use;

(2), alkaline chemical plating solution: take nickel sulfate, sodium hypophosphite, sodium citrate, anhydrous sodium acetate, sodium chloride, emulsifier OP-10, potassium iodate, dihexyl succinate sulfonic acid Sodium is dissolved in deionized water, and the pH is adjusted for later use;

4. First prepare the pickling solution in the pickling and rust removal process, then put the low carbon steel sheet into the pickling solution to pickle and remove rust, then perform mechanical polishing, take out the water for washing, and put it into the alkaline washing solution to remove oil after washing. , after degreasing, take it out and wash it with water, then carry out pickling activation, wash with water after activation, blow dry, put it in a pre-plating solution for surface pre-plating, and finally put it into an electroless plating solution for plating, rinse with water and dry after completion.

The present invention includes the following beneficial effects:

Compared with the prior art, the pearl nickel of the present invention has the advantages of good corrosion resistance, uniform coating, easier control and the like. The method of electroless pearl nickel plating developed in this paper has changed the single pearl nickel preparation method, with simpler operation, low cost, high utilization rate, saving resources, and achieving the advantages of economy and environmental protection.

Description of drawings

Figure 1 shows the appearance of nickel-plated products, in which a. bright nickel, b. semi-bright nickel, c. dark nickel, d. pearl nickel.

Figure 2 is a scanning electron microscope (SEM) image of pearl nickel (2000×).

Figure 3 is a scanning electron microscope (SEM) image of pearl nickel (10000×).

Detailed ways

The present invention will be further described below in conjunction with the best embodiments, but the protection scope of the present invention is not limited to the following embodiments.

Embodiment 1: The plating solution and method for electroless nickel plating of pearls of the present embodiment are carried out according to the following steps:

1. Preparation of alkaline washing solution: Dissolve sodium hydroxide, sodium phosphate, sodium silicate, sodium carbonate and sodium lauryl sulfate in deionized water for use;

2. Preparation of pre-plating solution: dissolve zinc oxide, zinc dihydrogen phosphate, phosphoric acid, citric acid, sodium fluoride, sodium dodecylbenzene sulfonate, and sodium molybdate in deionized water, adjust the pH, and stand by;

3. Preparation of chemical plating solution:

(1) Acid electroless plating solution: dissolve nickel sulfate, sodium hypophosphite, citric acid, anhydrous sodium acetate, sodium chloride, emulsifier OP-10, potassium iodate, sodium dihexyl succinate sulfonate In deionized water, adjust the pH for later use;

(2), alkaline chemical plating solution: take nickel sulfate, sodium hypophosphite, sodium citrate, anhydrous sodium acetate, sodium chloride, emulsifier OP-10, potassium iodate, dihexyl succinate sulfonic acid Sodium is dissolved in deionized water, and the pH is adjusted for later use;

4. First prepare the pickling solution in the pickling and rust removal process, then put the low carbon steel sheet into the pickling solution to pickle and remove rust, then perform mechanical polishing, take out the water for washing, and put it into the alkaline washing solution to remove oil after washing. , after degreasing, take it out and wash it with water, then carry out pickling activation, wash with water after activation, blow dry, put it in a pre-plating solution for surface pre-plating, and finally put it into an electroless plating solution for plating, rinse with water and dry after completion.

Embodiment 2: The difference between this embodiment and Embodiment 1 is that the degreasing process of the alkaline washing solution in step 1 is to remove the saponified grease through the saponification and emulsification of the lye, and the mechanism of infiltration and wetting to achieve degreasing. The purpose of the caustic washing liquid is sodium hydroxide 90g/L, sodium phosphate 30g/L, sodium silicate 20g/L, sodium carbonate 20g/L, sodium lauryl sulfate 0.02g/L, followed by adding deionized Dissolve in water. Others are the same as the first embodiment.

Embodiment 3: The difference between this embodiment and Embodiment 1 or 2 is that the formula of the pre-plating solution in step 2 and the surface pre-plating process are: preparing zinc oxide 12g/L, zinc dihydrogen phosphate 10g/L, Phosphoric acid 30mL/L, citric acid 0.5g/L, sodium fluoride 0.4g/L, sodium dodecylbenzenesulfonate 0.3g/L, sodium molybdate 1g/L 150ml solution in a 250mL beaker; put into the solution Concentrated ammonia water was added dropwise to adjust the pH to 2.5. Finally, the activated steel sheet was immersed in the treatment solution for reaction. After 15 min of reaction, it was taken out. The surface was rinsed with deionized water and dried for use. Others are the same as in the first or second embodiment.

Embodiment 4: The difference between this embodiment and Embodiments 1 to 3 is that the formula and process of the acid electroless plating bath described in step 3 are: preparing 100 mL of nickel sulfate 40g/L, sodium hypophosphite 50g/L, citric acid 20g/L, anhydrous sodium acetate 20g/L, sodium chloride 20g/L, emulsifier OP-10 2.4-4.8mL/L, potassium iodate 0.0005-0.001g/L, succinic acid A solution of 3.0 mL/L of sodium dihexyl sulfonate; add concentrated ammonia water dropwise to the solution to adjust pH to 4-4.5, heat the solution to 85-90 °C, put the pre-plated steel sheet into the plating solution, and perform plating After reaction for 1.5 h, rinse with deionized water and blow dry. Others are the same as one of Embodiments 1 to 3.

Embodiment 5: The difference between this embodiment and Embodiments 1 to 4 is that the formula and process of the alkaline electroless plating bath described in step 3 are: preparing 100 mL of nickel sulfate 40g/L, hypophosphorous acid Sodium 50g/L, sodium citrate 20g/L, anhydrous sodium acetate 20g/L, sodium chloride 20g/L, emulsifier OP-10 2.4-4.8mL/L, potassium iodate 0.0005-0.001g/L, A solution of 3.0 mL/L of sodium dihexyl sulfonate; add concentrated ammonia water dropwise to the solution to adjust the pH to 9-9.5, heat the solution to 40-60 °C, put the pre-plated steel sheet into the plating solution, and carry out The plating reaction was carried out for 1.5 h, and after removal, rinsed with deionized water and dried. Others are the same as one of Embodiments 1 to 4.

Embodiment 6: The difference between this embodiment and Embodiments 1 to 5 is that the pickling and rust removal solution and process in the low carbon steel pretreatment process described in step 4 are: the pickling solution is composed of deionized water and concentrated The hydrochloric acid is prepared in a volume ratio of 1:1, the pickling time is 5-10min, and the temperature is room temperature. Others are the same as one of Embodiments 1 to 5.

The content of the present invention is not limited to the content of the above-mentioned embodiments, and a combination of one or more specific embodiments can also achieve the purpose of the invention.

The beneficial effects of the present invention are verified by the following examples.

specific embodiment

A plating solution and method for chemically plating pearl nickel in the present embodiment is carried out according to the following steps:

1. Preparation of alkaline washing solution: Dissolve sodium hydroxide, sodium phosphate, sodium silicate, sodium carbonate and sodium lauryl sulfate in deionized water for use;

2. Preparation of pre-plating solution: dissolve zinc oxide, zinc dihydrogen phosphate, phosphoric acid, citric acid, sodium fluoride, sodium dodecylbenzene sulfonate, and sodium molybdate in deionized water, adjust the pH, and stand by;

3. Preparation of chemical plating solution:

(1) Acid electroless plating solution: dissolve nickel sulfate, sodium hypophosphite, citric acid, anhydrous sodium acetate, sodium chloride, emulsifier OP-10, potassium iodate, sodium dihexyl succinate sulfonate In deionized water, adjust the pH for later use;

(2), alkaline chemical plating solution: take nickel sulfate, sodium hypophosphite, sodium citrate, anhydrous sodium acetate, sodium chloride, emulsifier OP-10, potassium iodate, dihexyl succinate sulfonic acid Sodium is dissolved in deionized water, and the pH is adjusted for later use;

4. First prepare the pickling solution in the pickling and rust removal process, then put the low carbon steel sheet into the pickling solution to pickle and remove rust, then perform mechanical polishing, take out the water for washing, and put it into the alkaline washing solution to remove oil after washing. , after degreasing, take it out and wash it with water, then carry out pickling activation, wash with water after activation, blow dry, put it in a pre-plating solution for surface pre-plating, and finally put it into an electroless plating solution for plating, rinse with water and dry after completion.

The degreasing process of the alkaline washing solution described in this embodiment is to remove the saponified oil and grease through the saponification and emulsification of the alkaline solution and the mechanism of infiltration and wetting to achieve the purpose of degreasing. The formula of the alkaline washing solution is sodium hydroxide 90g/ L, sodium phosphate 30g/L, sodium silicate 20g/L, sodium carbonate 20g/L, and sodium lauryl sulfate 0.02g/L were added to deionized water in turn and dissolved.

The formula of the pre-plating solution and the surface pre-plating process described in this example are: preparing zinc oxide 12g/L, zinc dihydrogen phosphate 10g/L, phosphoric acid 30mL/L, citric acid 0.5g/L, sodium fluoride 0.4g/L g/L, sodium dodecylbenzenesulfonate 0.3g/L, sodium molybdate 1g/L 150ml solution in a 250mL beaker; add concentrated ammonia water dropwise to the solution, adjust pH to 2.5, and finally put the activated steel The tablets were immersed in the treatment solution for reaction, taken out after 15 min of reaction, rinsed with deionized water, and dried for use.

The formula and process of the acid electroless plating bath described in this embodiment are: preparing 100 mL containing 40g/L of nickel sulfate, 50g/L of sodium hypophosphite, 20g/L of citric acid, 20g/L of anhydrous sodium acetate, A solution of sodium chloride 20g/L, emulsifier OP-102.4-4.8mL/L, potassium iodate 0.0005-0.001g/L, sodium dihexyl succinate sulfonate 3.0mL/L; Adjust the pH to 4-4.5 with ammonia water, heat the solution to 85-90 °C, put the pre-plated steel sheet into the plating solution, carry out the plating reaction for 1.5 h, take it out, rinse with deionized water, and dry it.

The formula and process of the alkaline electroless plating bath described in this embodiment are: preparing 100 mL containing 40g/L of nickel sulfate, 50g/L of sodium hypophosphite, 20g/L of sodium citrate, and 20g/L of anhydrous sodium acetate. L, sodium chloride 20g/L, emulsifier OP-102.4-4.8mL/L, potassium iodate 0.0005-0.001g/L, sodium dihexyl succinate sulfonate 3.0mL/L solution; drop into the solution Add concentrated ammonia water to adjust the pH to 9-9.5, heat the solution to 40-60 ℃, put the pre-plated steel sheet into the plating solution, carry out the plating reaction for 1.5 h, take it out, rinse with deionized water, and blow dry.

The pickling and rust removal solution and process in the low carbon steel pretreatment process described in this embodiment are: the pickling solution is prepared by deionized water and concentrated hydrochloric acid in a volume ratio of 1:1, and the pickling time is 5-10min , the temperature is room temperature.

The appearance diagram and scanning electron microscope (SEM) of nickel pearls prepared in this example are shown in Figure 1, Figure 2, and Figure 3. The surface of nickel pearls obtained by the optimal formula is uniform and dense, with pearl-like texture and jade-like luster. .

The preparation process adopted in the example of this case is simple in operation, simple in process, energy-saving and environmentally friendly, and changes the single preparation process of pearl nickel.

The test result of the corrosion resistance of the pearl nickel prepared in this example is that the corrosion resistance of the pearl nickel is tested with a copper sulfate solution of 41 g/L, and no rust spots appear in an average of 3 hours.

Claims (4)

1. A method for chemically plating pearl nickel is characterized by comprising the following steps: the method comprises the following steps:

firstly, preparing an alkaline washing solution: dissolving sodium hydroxide, sodium phosphate, sodium silicate, sodium carbonate and sodium dodecyl sulfate in deionized water for later use;

secondly, preparing a pre-plating solution: dissolving zinc oxide, zinc dihydrogen phosphate, phosphoric acid, citric acid, sodium fluoride, sodium dodecyl benzene sulfonate and sodium molybdate in deionized water, and adjusting the pH value for later use;

preparing chemical plating solution, wherein the chemical plating solution is acidic chemical plating solution or alkaline chemical plating solution

(1) Acid electroless plating solution: dissolving nickel sulfate, sodium hypophosphite, citric acid, anhydrous sodium acetate, sodium chloride, an emulsifier OP-10, potassium iodate and sodium dihexyl succinate sulfonate in deionized water, and adjusting the pH value for later use;

(2) alkaline electroless plating solution: dissolving nickel sulfate, sodium hypophosphite, sodium citrate, anhydrous sodium acetate, sodium chloride, an emulsifier OP-10, potassium iodate and sodium dihexyl succinate sulfonate in deionized water, and adjusting the pH value for later use;

fourthly, firstly preparing a pickling solution in a pickling and rust removing process, then putting the low-carbon steel sheet into the pickling solution for pickling and rust removing, then performing mechanical polishing, taking out and washing, after washing, putting into an alkali washing solution for oil removal, after oil removal, taking out and washing, then performing pickling and activation, after activation, washing, drying, putting into a pre-plating solution for surface pre-plating, finally putting into a chemical plating solution for plating, after completion, washing and drying;

the preparation process of the acidic electroless plating solution comprises the following steps: preparing 100mL of solution containing 40g/L of nickel sulfate, 50g/L of sodium hypophosphite, 20g/L of citric acid, 20g/L of anhydrous sodium acetate, 20g/L of sodium chloride, 102.4-4.8 mL/L of emulsifier OP-0.0005-0.001 g/L of potassium iodate and 3.0mL/L of dihexyl sodium sulfosuccinate; dropwise adding concentrated ammonia water into the solution to adjust the pH value to 4-4.5, heating the solution to 85-90 ℃, putting the steel sheet with the pre-plated surface into a plating solution, performing plating reaction for 1.5h, taking out, washing with deionized water, and drying;

the preparation process of the alkaline chemical plating solution comprises the following steps: preparing 100mL of solution containing 40g/L of nickel sulfate, 50g/L of sodium hypophosphite, 20g/L of sodium citrate, 20g/L of anhydrous sodium acetate, 20g/L of sodium chloride, 102.4-4.8 mL/L of emulsifier OP-0.0005-0.001 g/L of potassium iodate and 3.0mL/L of dihexyl sodium sulfosuccinate; dropwise adding concentrated ammonia water into the solution to adjust the pH value to 9-9.5, heating the solution to 40-60 ℃, putting the steel sheet with the pre-plated surface into a plating solution, performing plating reaction for 1.5h, taking out, washing with deionized water, and drying.

2. The method of claim 1, wherein: the alkali wash oil removal process is to remove saponifiable oil through the mechanisms of saponification, emulsification and soaking and wetting of alkali liquor to achieve the purpose of oil removal, and the formula of the alkali wash is that 90g/L of sodium hydroxide, 30g/L of sodium phosphate, 20g/L of sodium silicate, 20g/L of sodium carbonate and 0.02g/L of sodium dodecyl sulfate are sequentially added into deionized water to be dissolved.

3. The method of claim 1, wherein: the preparation and surface pre-plating process of the pre-plating solution comprises the following steps: preparing 150mL solution of 12g/L zinc oxide, 10g/L zinc dihydrogen phosphate, 30mL/L phosphoric acid, 0.5g/L citric acid, 0.4g/L sodium fluoride, 0.3g/L sodium dodecyl benzene sulfonate and 1g/L sodium molybdate in a 250mL beaker; dropwise adding concentrated ammonia water into the solution, adjusting the pH value to 2.5, finally immersing the activated steel sheet into the treatment solution for reaction, taking out after 15min of reaction, washing the surface with deionized water after taking out, and drying for later use.

4. The method of claim 1, wherein: the pickling solution and the process in the low-carbon steel sheet pickling and derusting process are as follows: the pickling solution is prepared from deionized water and concentrated hydrochloric acid according to the volume ratio of 1:1, the pickling time is 5-10min, and the temperature is room temperature.

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