阅读说明：本技术 一种镍基复合镀层的节能制备方法 (Energy-saving preparation method of nickel-based composite coating ) 是由 杨树华 崔砚伟 付文清 曹丙强 于 2021-07-30 设计创作，主要内容包括：本发明涉及一种镍基复合镀层的节能制备方法。该方法具体制备工艺步骤如下：将不同比例的还原剂和第二相加入电镀液中,随后在不同的电镀工艺参数下,通过电镀获得镍基复合镀层。本发明通过在电镀液中加入还原剂和第二相,可以同时实现耐蚀性的提升和电镀能耗的降低。(The invention relates to an energy-saving preparation method of a nickel-based composite coating. The method comprises the following specific preparation process steps: adding reducing agents and second phases with different proportions into the electroplating solution, and then obtaining the nickel-based composite coating through electroplating under different electroplating process parameters. According to the invention, the reducing agent and the second phase are added into the electroplating solution, so that the corrosion resistance can be improved and the electroplating energy consumption can be reduced.)

1. An energy-saving preparation method of a nickel-based composite coating is characterized in that the formula comprises 200-300 g/L of nickel sulfate, 30-60 g/L of nickel chloride, 20-50 g/L of boric acid, 5-15 g/L of a softening agent, 3-8 g/L of a main light agent, 1-5 g/L of a wetting agent, 4-20 g/L of a second phase and 0.8-4 g/L of a reducing agent, and the solvent is deionized water;

the softening agent is selected from one or more of saccharin and ALS (sodium allylsulfonate);

the main light agent is selected from one or more of 1, 4-butynediol, PPS (pyriminum propanesulfonate) and benzylidene acetone;

the wetting agent is selected from one or more of sodium dodecyl sulfate, sodium isooctyl sulfate and polyethylene glycol;

the second phase is selected from Al₂O₃、TiO₂、ZrO₂、SiO₂、CeO₂One of or of SiCSeveral kinds of the raw materials;

the reducing agent is selected from one or more of sodium hypophosphite, sodium borohydride, borane and hydrazine;

the energy-saving preparation method of the nickel-based composite coating comprises the following steps:

the method comprises the following steps: respectively weighing nickel sulfate, nickel chloride, boric acid, a second phase, a reducing agent, a softening agent, a main light agent and a wetting agent, and dissolving into deionized water to obtain a plating solution;

step two: pretreating a base material;

step three: heating the plating solution;

step four: putting the substrate material into the plating solution and standing for a period of time;

step five: electroplating to obtain the nickel-based plating layer.

2. The energy-saving preparation method of the nickel-based composite coating according to claim 1, wherein the base material in the second step is one of a copper sheet, a stainless steel sheet, a Q35 carbon steel sheet and an aluminum sheet.

3. The energy-saving preparation method of the nickel-based composite coating according to claim 1, wherein the temperature of the coating in the third step is 50-60 ℃.

4. The energy-saving preparation method of the nickel-based composite coating according to claim 1, wherein the standing time of the base material in the plating solution in the fourth step is 1-15 min.

5. The energy-saving preparation method of the nickel-based composite coating according to claim 1, wherein the electroplating time in the fifth step is 1-20 min, and the current density is 0.2A/dm²~10.2 A/dm²。

Technical Field

The invention relates to the field of nickel electroplating, in particular to an energy-saving preparation method of a nickel-based composite coating.

Background

Composite electroplating is a new surface strengthening process for obtaining composite material, and is characterized by that it adds one or several insoluble microparticles with a certain property into the plating solution, and uniformly disperses them in the plating solution by various modes, and makes them inlaid and codeposited with metal so as to obtain the composite plating layer with special properties and functional material. Among them, the nickel-based composite plating layer has better functions of wear resistance, corrosion resistance, high temperature oxidation resistance and the like, and is considered as an effective method for improving the performance of the plating layer. At present, most of nickel-based composite coatings improve the corrosion resistance of the coating by adding a second phase such as alumina, silicon carbide, tungsten carbide, silica, titanium dioxide and the like into a nickel plating solution. However, the research mainly focuses on the regulation and control of the type of the second phase, the particle size of the second phase and the addition amount of the second phase, and the research focuses on the energy consumption problem of the nickel electroplating, and the energy consumption problem of the nickel electroplating not only can reduce the production cost of the nickel electroplating industry, but also has important significance on environmental protection. Therefore, on the basis of ensuring the corrosion resistance of the nickel-based composite plating layer, the development of the energy-saving preparation method of the nickel-based composite plating layer has great significance.

Disclosure of Invention

On the basis of the prior art, the invention provides an energy-saving preparation method of a nickel-based composite coating. The existing research on the nickel-based composite plating layer mainly focuses on the regulation and control of the type of the second phase, the particle size of the second phase and the addition amount of the second phase, and few researches focus on the energy consumption problem of the nickel electroplating, so that the invention promotes the electrochemical process by adding the second phase and a reducing agent into a typical Watt plating solution through chemical reduction, thereby achieving the effect of saving energy consumption on the basis of ensuring the corrosion resistance of the nickel-based composite plating layer.

The purpose of saving energy consumption in the preparation of the nickel-based composite plating layer is achieved on the basis of ensuring the corrosion resistance of the nickel-based composite plating layer. The invention provides an energy-saving preparation method of a nickel-based composite plating layer, which realizes chemical reduction to promote electrochemical reduction by adding a second phase and a reducing agent into a nickel plating solution, and realizes the energy-saving effect on the basis of ensuring the corrosion resistance of the nickel-based composite plating layer.

The purpose of the invention is mainly realized by the following technical scheme:

the invention provides an energy-saving preparation method of a nickel-based composite coating, wherein the plating solution comprises 200-300 g/L of nickel sulfate, 30-60 g/L of nickel chloride, 20-50 g/L of boric acid, 5-15 g/L of a softening agent, 3-8 g/L of a main light agent, 1-5 g/L of a wetting agent, 4-20 g/L of a second phase and 0.8-4 g/L of a reducing agent. The solvent is deionized water.

The invention provides an energy-saving preparation method of a nickel-based composite coating, which comprises the following steps:

the method comprises the following steps: respectively weighing nickel sulfate, nickel chloride, boric acid, a second phase, a reducing agent, a softening agent, a main light agent and a wetting agent, and dissolving into deionized water to obtain a plating solution;

step two: pretreating a base material;

step three: heating the plating solution;

step four: putting the substrate material into the plating solution and standing for a period of time;

step five: electroplating to obtain the nickel-based composite coating.

Further, the base material is one of a copper sheet, a stainless steel sheet, a Q35 carbon steel sheet and an aluminum sheet;

further, the temperature of the plating solution is 50-60 ℃;

further, the standing time in the fourth step is 1-15 min;

further, in the fifth step, the electroplating time is 1-20 min;

further, the current density in the fifth step is 0.2A/dm²~10.2 A/dm²。

Compared with the prior art, the invention can realize at least one of the following beneficial effects:

(a) according to the energy-saving preparation method of the nickel-based composite coating, the prepared basic plating solution has higher concentration of main salt and higher temperature of the bath solution, so that the plating solution has high conductivity, various ions have high moving speed, and better covering capacity and dispersing capacity, thereby improving the electroplating efficiency and having higher process value;

(b) according to the energy-saving preparation method of the nickel-based composite coating, the added solid particles in the second phase can influence the crystallization process of the nickel grains, so that the dispersion strengthening effect is achieved, the nickel grains are refined, the electrochemical deposition process is promoted, the energy-saving effect is achieved, the added second phase generally has higher hardness and physical and chemical properties similar to those of a metal matrix, and the corrosion resistance of the nickel-based composite coating is improved. The corrosion resistance is improved and the electroplating energy consumption is reduced at the same time;

(c) according to the energy-saving preparation method of the nickel-based composite coating, provided by the invention, nickel ions are rapidly nucleated by adding the reducing agent and utilizing the strong reduction effect of the reducing agent to form a thin chemical deposition layer mainly based on chemical reaction, the deposition layer has catalytic activity on the surface of a substrate, the cathodic electrochemical deposition reaction is promoted, and the electrochemical deposition plays a leading role along with the slow progress of the chemical reaction. Therefore, the alloy coating obtained by the synergistic effect of the chemical reduction and the electrochemical reduction plays a role in saving energy consumption in industrial production;

(d) according to the energy-saving preparation method of the nickel-based composite plating layer, the second phase is added into the basic plating solution, and the adjustment and matching of the amount of the reducing agent are realized, so that the corrosion resistance can be improved, and the electroplating energy consumption can be reduced.

Drawings

The drawings are only for purposes of illustrating particular embodiments and are not to be construed as limiting the invention.

FIG. 1 is a polarization curve of the nickel-based composite plating layer prepared in example 1.

Fig. 2 is a linear voltammogram of the nickel-based composite plating solution prepared in example 1.

Detailed Description

Preferred embodiments of the present invention will now be described in detail with reference to the accompanying drawings, which form a part hereof, and which illustrate, by way of example, the present invention.

Example 1

(1) Preparing a basic plating solution, weighing 70 g of nickel sulfate, 12.5 g of nickel chloride and 11.25 g of boric acid, then weighing 2.5 g of saccharin, 1 g of 1, 4-butynediol and 1.25 g of polyethylene glycol, and putting the above reagents into a 250 ml beaker;

(2) adding 2g of Al into the beaker in the step 1₂O₃And 0.2 g of sodium hypophosphite. Water was then added to the beaker to 250 ml and stirred thoroughly with a magnetic stirrer until all dissolved. Thus obtaining the plating solution;

(3) and cleaning the Hull cell by using deionized water and drying. In addition, the copper sheets and the nickel blocks are polished by sand paper and washed by ultrasonic waves;

(4) carrying out an electroplating experiment in a Hull cell, and preparing a constant-current power supply, a water bath, an ultrasonic cleaner and the like of an electroplating instrument;

(5) heating the prepared plating solution in water bath at 55 ℃;

(6) placing the copper sheet into the plating solution and standing for 8 min;

(7) the nickel block is placed at the right-angle end of the Hull cell to serve as an anode and connected with a positive electrode of a power supply, and the copper sheet is placed at the inclined-plane end to serve as a cathode and connected with a negative electrode of the power supply for electroplating. Electroplating time is 9 min, and current density is 0.2A/dm². Finally, the nickel-based composite plating layer is obtained.

The polarization curve (figure 1) of the nickel-based composite plating layer obtained by the nickel-based composite plating layer prepared in the example 1 and the standard Watt plating solution (the nickel-based composite plating solution in the step 1 of the example 1) can show that the corrosion current of the nickel-based composite plating layer prepared in the example 1 is reduced by 17.24 muA, namely reduced by 74.9 percent, so that the corrosion resistance is obviously improved, in addition, the linear voltammetry curve (figure 2) obtained by the nickel-based composite plating solution prepared in the example 1 and the standard Watt plating solution (the nickel-based composite plating solution in the step 1 of the example 1) can show that the reduction potential of nickel ions in the plating solution in the example 1 is obviously reduced relative to the standard Watt plating solution (the nickel-based composite plating solution in the step 1 of the example 1), so that the electroplating energy consumption is obviously reduced, so that the energy-saving effect achieved by the method is very obvious,

in conclusion, the reducing agent and the second phase are added into the plating solution, so that the corrosion resistance can be improved and the energy consumption of electroplating can be reduced at the same time.

Example 2

(1) Preparing a basic plating solution, namely weighing 50 g of nickel sulfate, 15 g of nickel chloride and 10 g of boric acid, then weighing 2g of saccharin, 1 g of PPS (pyritinoin propanesulfonate) and 1 g of sodium dodecyl sulfate, and putting the above reagents into a 250 ml beaker;

(2) 2g of TiO was added to the beaker in step 1₂And 5 g of sodium hypophosphite. Water was then added to the beaker to 250 ml and stirred thoroughly with a magnetic stirrer until all dissolved. Thus obtaining the plating solution;

(3) and cleaning the Hull cell by using deionized water and drying. In addition, the stainless steel sheet and the nickel block are polished by sand paper and washed by ultrasonic waves;

(4) carrying out an electroplating experiment in a Hull cell, and preparing a constant-current power supply, a water bath, an ultrasonic cleaner and the like of an electroplating instrument;

(5) heating the prepared plating solution in water bath at 55 ℃;

(6) placing the stainless steel sheet in a plating solution and standing for 10 min;

(7) the nickel block is placed at the right-angle end of the Hull cell to serve as the anode to be connected with the positive electrode of a power supply, and the stainless steel sheet is placed at the inclined-plane end to serve as the cathode to be connected with the negative electrode of the power supply for electroplating. The electroplating time is 9 min, and the current density is 2.8A/dm². Finally, the nickel-based composite plating layer is obtained.

Example 3

(1) Preparing a basic plating solution, namely weighing 50 g of nickel sulfate, 7.5 g of nickel chloride and 5 g of boric acid, then weighing 3 g of ALS (sodium allylsulfonate), 1.5 g of PPS (pyriminum propanesulfonate) and 1.25 g of sodium isooctyl sulfate, and putting the above reagents into a 250 ml beaker together;

(2) adding 4 g of SiO into the beaker in the step 1₂And 2.5 g of borane. Water was then added to the beaker to 250 ml and stirred thoroughly with a magnetic stirrer until all dissolved. Thus obtaining the plating solution;

(3) and cleaning the Hull cell by using deionized water and drying. Polishing the Q35 carbon steel sheet and the nickel block by using sand paper, and washing by using ultrasonic waves;

(4) carrying out an electroplating experiment in a Hull cell, and preparing a constant-current power supply, a water bath, an ultrasonic cleaner and the like of an electroplating instrument;

(5) heating the prepared plating solution in water bath at 60 ℃;

(6) putting the Q35 carbon steel sheet into the plating solution and standing for 15 min;

(7) the nickel block is placed at the right-angle end of the Hull cell to serve as the anode to be connected with the positive electrode of a power supply, and the Q35 carbon steel sheet is placed at the inclined-plane end to serve as the cathode to be connected with the negative electrode of the power supply for electroplating. The electroplating time is 10 min, and the current density is 5.6A/dm². Finally, the nickel-based composite plating layer is obtained.

Example 4

(1) Preparing basic plating solution, weighing 75 g of nickel sulfate, 15 g of nickel chloride and 12.5 g of boric acid, then weighing 3 g of saccharin, 2g of benzalacetone and 1.25 g of polyethylene glycol, and putting the above reagents into a 250 ml beaker;

(2) 2g of SiC and 0.2 g of sodium hypophosphite were added to the beaker from step 1. Water was then added to the beaker to 250 ml and stirred thoroughly with a magnetic stirrer until all dissolved. Thus obtaining the plating solution;

(3) and cleaning the Hull cell by using deionized water and drying. In addition, the copper sheets and the nickel blocks are polished by sand paper and washed by ultrasonic waves;

(4) carrying out an electroplating experiment in a Hull cell, and preparing a constant-current power supply, a water bath, an ultrasonic cleaner and the like of an electroplating instrument;

(5) heating the prepared plating solution in water bath at 50 ℃;

(6) placing the aluminum sheet into the plating solution and standing for 2 min;

(7) the nickel block is placed at the right-angle end of the Hull cell and used as the anode to be connected with the positive electrode of the power supply, and the aluminum sheet is placed at the inclined-plane end and used as the cathode to be connected with the negative electrode of the power supply for electroplating. The electroplating time is 8 min, and the current density is 10.2A/dm². Finally, the nickel-based composite plating layer is obtained.

Example 5

(1) Preparing basic plating solution, weighing 75 g of nickel sulfate, 7.5 g of nickel chloride and 5 g of boric acid, then weighing 2.5 g of saccharin, 1 g of benzalacetone and 1.25 g of polyethylene glycol, and putting the above reagents into a 250 ml beaker;

(2) 4 g of SiC and 3 g of sodium borohydride were added to the beaker in step 1. Water was then added to the beaker to 250 ml and stirred thoroughly with a magnetic stirrer until all dissolved. Thus obtaining the plating solution;

(3) and cleaning the Hull cell by using deionized water and drying. In addition, polishing the aluminum sheets and the nickel blocks by using sand paper, and washing by using ultrasonic waves;

(4) carrying out an electroplating experiment in a Hull cell, and preparing a constant-current power supply, a water bath, an ultrasonic cleaner and the like of an electroplating instrument;

(5) heating the prepared plating solution in water bath at 50 ℃;

(6) placing the aluminum sheet into the plating solution and standing for 10 min;

(7) the nickel block is placed at the right-angle end of the Hull cell and used as the anode to be connected with the positive electrode of the power supply, and the aluminum sheet is placed at the inclined-plane end and used as the cathode to be connected with the negative electrode of the power supply for electroplating. The electroplating time is 15 min, and the current density is 10.2A/dm². Finally, the nickel-based composite plating layer is obtained.

The above description is only a partial preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are included in the scope of the present invention.