CN108570696B - High-current-density-resistant acidic zinc-nickel electroplating solution and application thereof - Google Patents
High-current-density-resistant acidic zinc-nickel electroplating solution and application thereof Download PDFInfo
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- CN108570696B CN108570696B CN201810361101.XA CN201810361101A CN108570696B CN 108570696 B CN108570696 B CN 108570696B CN 201810361101 A CN201810361101 A CN 201810361101A CN 108570696 B CN108570696 B CN 108570696B
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- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/565—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of zinc
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Abstract
The invention discloses a high-current-density-resistant acidic zinc-nickel electroplating solution and application thereof. Such high current resistanceThe acid zinc-nickel electroplating solution with the density consists of the following raw materials: zinc chloride, nickel chloride, alcohol amine compounds, conductive salt, a pH buffering agent, a brightening agent, a complexing agent and water. Also discloses a method for electroplating by using the acid zinc-nickel electroplating solution with high current density resistance. The high-current-density-resistant acidic zinc-nickel electroplating solution does not contain ammonium chloride, reduces the difficulty in wastewater treatment, adopts a novel composite additive, has good wettability and low foaming performance, does not influence normal production even if an air stirring and continuous filtering device is adopted, and is 0-3A/dm2Within a wider current density range, the nickel content of the coating can be stabilized within a certain range, the uniformity of the nickel content in the coating in high and low regions is well improved, and the nickel content can bear more than 5A/dm2The current density is also not easily scorched.
Description
Technical Field
The invention relates to a high-current-density-resistant acidic zinc-nickel electroplating solution and application thereof.
Background
For the protection of automobile parts, the traditional method is to carry out galvanizing on the surface of the automobile parts, but the corrosion rate of the galvanized layer is too high, and particularly, the traditional galvanized layer cannot meet the requirement along with the increasing requirement of the automobile parts on corrosion resistance. The zinc-nickel alloy electroplating is used as a substitute, the corrosion resistance of a zinc-nickel alloy coating is excellent, the zinc-nickel alloy coating is more than 5 times that of a zinc coating under the same condition, the hydrogen brittleness sensitivity is low, and the weldability and the toughness have great advantages. The electroplated zinc-nickel alloy mainly has an acidic solution system and an alkaline solution system, the alkaline system has good dispersion performance, the electroplated alloy has uniform components in a large current density range, but the electroplated zinc-nickel alloy has low current efficiency, is easy to cause hydrogen embrittlement when used, has large smell in the implementation process, is difficult to control the electroplating solution, has an aging phenomenon, and is difficult to treat discharged wastewater. The acid system has the advantages of high current efficiency, 50 percent lower cost than the alkaline system, less hydrogen embrittlement on steel substrates, simple treatment of electroplating sewage, no aging phenomenon of the plating solution and the like. Thus, the development of acidic systems is rapid.
However, the current acidic solution systems have the following significant drawbacks: (1) in the plating process, ammonium chloride is commonly used for keeping the pH value and the conductivity of the solution, so that the difficulty of wastewater treatment is increased; (2) the plating process generally adopts an air stirring and continuous filtering device and plating solutionA large amount of foam layers are generated on the surface, so that the foam layers overflow the plating tank and the production is seriously influenced; (3) in the electroplating process, the proportion of nickel in the coating in the high and low current areas is not uniform, and when the current density is more than 4A/dm2Even scorching occurs at high current densities.
Disclosure of Invention
The invention aims to provide an acid zinc-nickel electroplating solution with high current density resistance and application thereof aiming at the defects of the prior acid zinc-nickel alloy, and the electroplating solution can be used at 0-3A/dm2Electroplating is carried out within a wide current density range, the proportion of the nickel content in the coating is uniform, and the coating can bear more than 5A/dm2The current density is not scorched.
The technical scheme adopted by the invention is as follows:
a high-current-density-resistant acidic zinc-nickel electroplating solution is composed of the following raw materials:
in the acid zinc-nickel electroplating solution with high current density resistance, the structural general formula of the alcohol amine compound is as follows:
in the general formula, R1H or an alkyl group having C1 to C4; r2Represents H, -CH3、-CH2OH、-CH2CH2OH、-CH2NH2、-CH2CH2NH2；R3Represents an alkylene group having a carbon number of 1 to 5.
In the acid zinc-nickel electroplating solution with high current density resistance, the conductive salt is at least one of potassium chloride, sodium chloride, potassium sulfate and sodium sulfate.
In the acidic zinc-nickel electroplating solution with high current density resistance, the pH buffering agent is at least one of boric acid, borate, acetic acid, acetate, citric acid and citrate.
In the acid zinc-nickel electroplating solution with high current density resistance, the brightener is at least one of benzalacetone, dibenzylidene acetone, aromatic acetone, methyl naphthylacetone, o-chlorocinnamic acid, o-chlorobenzaldehyde, cinnamic acid, coumarin, polyethylene glycol and triethanolamine.
In the acid zinc-nickel electroplating solution with high current density resistance, the complexing agent is at least one of malic acid, gluconic acid, sodium tartrate, sodium citrate, sodium gluconate, potassium tartrate, potassium citrate, potassium gluconate, ammonium tartrate, ammonium malate, ammonium citrate, ammonium gluconate, monoethanolamine, triethylenetetramine and tetraethylenepentamine.
The method for electroplating zinc and nickel is to use the acid zinc and nickel electroplating solution with high current density resistance to electroplate a substrate.
The invention has the beneficial effects that:
the high-current-density-resistant acidic zinc-nickel electroplating solution does not contain ammonium chloride, reduces the difficulty in wastewater treatment, adopts a novel composite additive, has good wettability and low foaming performance, does not influence normal production even if an air stirring and continuous filtering device is adopted, and is 0-3A/dm2Within a wider current density range, the nickel content of the coating can be stabilized within a certain range, the uniformity of the nickel content in the coating in high and low regions is well improved, and the nickel content can bear more than 5A/dm2The current density is also not easily scorched.
The method comprises the following specific steps:
1. the electroplating solution does not contain ammonium chloride, so that the treatment difficulty of the wastewater is reduced, and a large amount of cost is saved for enterprises;
2. the various additives adopted by the invention have excellent performance and better wetting performance, and a large amount of bubbles can not be generated even under the conditions of air stirring and connection of a filtering device;
3. the technical effect of the additive containing the alcohol amine compound is to improve the uneven proportion of the nickel content in the coating and ensure that the nickel content in the coating is 0-3A/dm2The wide current density range is kept in a stable state and can bear more than 5A/dm2The high current of (2) does not scorch and shows excellent performance.
Detailed Description
A high-current-density-resistant acidic zinc-nickel electroplating solution is composed of the following raw materials:
more preferably, the acid zinc-nickel electroplating solution resistant to high current density comprises the following raw materials:
preferably, in the acidic zinc-nickel electroplating solution with high current density resistance, the structural general formula of the alcohol amine compound is as follows:
in the general formula, R1H or an alkyl group having C1 to C4; r2Represents H, -CH3、- CH2OH、-CH2CH2OH、-CH2NH2、-CH2CH2NH2；R3An alkylene group having a carbon number of 1 to 5; the alkyl or alkylene is a straight chain or branched alkyl chain; further preferably, in the formula, R1Represents H, methyl, ethyl, n-propyl or isopropyl, R2Represents H, -CH2OH or-CH2CH2OH，R3Represents a methylene group or an ethylene group.
Preferably, in the high current density resistant acidic zinc-nickel electroplating solution, the conductive salt is at least one of potassium chloride, sodium chloride, potassium sulfate and sodium sulfate.
Preferably, in the acidic zinc-nickel plating solution resistant to high current density, the pH buffer is at least one of boric acid, borate, acetic acid, acetate, citric acid and citrate.
Preferably, in the acidic zinc-nickel electroplating solution resistant to high current density, the brightener is at least one of benzalacetone, dibenzylidene acetone, aromatic acetone, methyl naphthylethanone, methyl naphthylacetone, o-chlorocinnamic acid, o-chlorobenzaldehyde, cinnamic acid, coumarin, polyethylene glycol and triethanolamine.
Preferably, in the high current density resistant acidic zinc-nickel electroplating solution, the complexing agent is at least one of malic acid, gluconic acid, sodium tartrate, sodium citrate, sodium gluconate, potassium tartrate, potassium citrate, potassium gluconate, ammonium tartrate, ammonium malate, ammonium citrate, ammonium gluconate, monoethanolamine, triethylenetetramine and tetraethylenepentamine.
The method for electroplating zinc and nickel is to use the acid zinc and nickel electroplating solution with high current density resistance to electroplate a substrate.
The electroplating method comprises the following steps: chemical high-temperature degreasing → washing → anode electrolysis → washing → acid washing → ultrasonic degreasing → washing → anode electrolysis → washing → hydrochloric acid activation → washing → electroplating acidic zinc nickel → washing → passivation → washing → sealing → drying.
Preferably, in the method for electroplating zinc and nickel, the electroplating parameters are as follows: current density of 0-3A/dm2(not 0A), the pH value is 5.2-5.8, the electroplating time is 30-60 min, and the electroplating temperature is 30-40 ℃.
The present invention will be described in further detail with reference to specific examples. The starting materials used in the examples are, unless otherwise specified, commercially available from conventional sources.
Example 1:
the high current density resistant acidic zinc-nickel electroplating bath of example 1 was comprised of the following raw materials: 40g/L of zinc chloride, 90g/L of nickel chloride, 200g/L of conductive salt, 60g/L of pH buffering agent, 1mL/L of brightening agent, 12mL/L of complexing agent and 10g/L of alcohol amine compound (R in the general formula of alcohol amine compound)1Is H, R2is-CH2OH，R3Ethylene) and the balance of distilled water.
The raw materials for the conductive salt, pH buffer, brightener and complexing agent are those disclosed above, which are conventional in the art. The compositions of the conductive salt, the pH buffer, the brightener and the complexing agent used in the examples of the invention and the comparative examples were the same.
Comparative example 1:
the zinc-nickel electroplating bath of comparative example 1 consisted of the following raw materials: 40g/L of zinc chloride, 90g/L of nickel chloride, 200g/L of conductive salt, 60g/L of pH buffering agent, 1mL/L of brightening agent, 12mL/L of complexing agent and the balance of distilled water.
Example 2:
the high current density resistant acidic zinc-nickel electroplating bath of example 2 was comprised of the following raw materials: 50g/L of zinc chloride, 100g/L of nickel chloride, 210g/L of conductive salt, 50g/L of pH buffer agent, 1mL/L of brightening agent, 12mL/L of complexing agent and 10g/L of alcohol amine compound (R in the general formula of alcohol amine compound)1Is H, R2is-CH2OH，R3Ethylene) and the balance of distilled water.
Comparative example 2:
the zinc-nickel electroplating bath of comparative example 2 consisted of the following raw materials: 50g/L of zinc chloride, 100g/L of nickel chloride, 210g/L of conductive salt, 50g/L of pH buffer, 1mL/L of brightener, 12mL/L of complexing agent and the balance of distilled water.
Application example 1:
the plating test was carried out in a 267mL Hull cell using the zinc-nickel plating solution of example 1, the substrate material being standard steel with dimensions of 100mm x 60mm, the plating conditions being a current density of 1A, a plating time of 10min, a temperature of 35 ℃ and a pH of 5.4.
The nickel content of the coating was determined using an XDL X-ray fluorescence coating thickness gauge (Fischer, Germany). Drawing a straight line by using the central line of the horizontal plane of the standard sheet, and respectively measuring the nickel content of 2cm, 4cm, 6cm, 8cm and 9cm by using the left boundary as a starting point so as to know the nickel content of the plating layer in the current high and low regions. Meanwhile, the current at the position of 1cm with the left boundary of the standard sheet as the starting point is observed to be 5.1A/dm2The plating state and the bubble generation of the plating solution in the inflated state.
The results show that: from the state of aeration during the plating, the plating solution generated very little bubbles, confirming that the plating solution has low bubble properties. The brightness of all the areas of the standard sheet is high, and the phenomenon of scorching does not exist. The nickel content in the plating layers of different current areas of the standard sheet is shown in table 1, and the nickel content in the high-low current areas is quite uniform.
TABLE 1 results of plating in example 1
| L (distance cm to the leftmost side of the standard sheet) | Nickel content (wt%) of plating layer |
| 2 | 13.2 |
| 4 | 12.7 |
| 6 | 13.1 |
| 8 | 12.6 |
| 9 | 14.1 |
Application comparative example 1:
electroplating was carried out using the zinc-nickel plating solution of comparative example 1 in the same manner as in application example 1.
The results show that: from the state of aeration during the plating, the plating solution generated very little bubbles, confirming that the plating solution has low bubble properties. The brightness of the standard film is observed to be high, but the left side of the standard film with the left boundary being the starting point of 1cm has a slight scorching phenomenon. The nickel content in the plating layer of the standard sheet in different current areas is shown in table 2, and the nickel content in high and low current areas is quite uneven.
TABLE 2 electroplating results of comparative example 1
| L (distance cm to the leftmost side of the standard sheet) | Nickel content (wt%) of plating layer |
| 2 | 11.2 |
| 4 | 13.2 |
| 6 | 9.8 |
| 8 | 16.6 |
| 9 | 19.1 |
Application example 2:
electroplating was carried out using the zinc-nickel plating solution of example 2 in the same manner as in application example 1.
The results show that: from the aeration state in the electroplating process, the plating solution generates less bubbles, and the plating solution is proved to have low-bubble performance. The brightness of all the areas of the standard sheet is high, and the phenomenon of scorching does not exist. The nickel content in the plating layer of the standard sheet in different current areas is shown in table 3, and the nickel content in the high and low current areas is quite uniform.
TABLE 3 results of plating of example 2
| L (distance criterion)Distance cm to the leftmost side of the sheet) | Nickel content (wt%) of plating layer |
| 2 | 12.6 |
| 4 | 12.7 |
| 6 | 12.1 |
| 8 | 13.7 |
| 9 | 13.4 |
Application comparative example 2:
the plating was carried out using the zinc-nickel plating solution of comparative example 2 in the same manner as in application example 1.
The results show that: from the aeration state in the electroplating process, the plating solution generates less bubbles, and the plating solution is proved to have low-bubble performance. The brightness of the standard film is observed to be high, but the left side of the standard film with the left boundary being the starting point of 1cm has a slight scorching phenomenon. The nickel content in the plating layer of the standard sheet in different current areas is shown in table 4, and the nickel content in high and low current areas is quite uneven.
TABLE 4 results of plating of comparative example 2
| L (distance cm to the leftmost side of the standard sheet) | Nickel content (wt%) of plating layer |
| 2 | 10.4 |
| 4 | 12.7 |
| 6 | 11.8 |
| 8 | 15.7 |
| 9 | 18.4 |
Compared with the prior art, the invention has the following advantages:
1. the electroplating solution does not contain ammonium chloride, so that the treatment difficulty of the wastewater is reduced.
2. The novel composite additive is adopted, so that the coating has good wettability and low foaming performance, and even if air stirring and connection of a filtering device are adopted, the plating solution cannot overflow the plating tank to influence normal production.
3. At 0 to 3A/dm2Within a wide current density range, the proportion of the nickel content in the coating is uniform and can bear more than 5A/dm2The current density is not scorched.
Claims (5)
1. The acid zinc-nickel electroplating solution with high current density resistance is characterized in that: the feed consists of the following raw materials:
the structural formula of the alcohol amine compound is as follows:
R1is a compound of formula (I) in the formula (H),R2is-CH2OH，R3Is an ethylene group;
the complexing agent is at least one of malic acid, gluconic acid, sodium tartrate, sodium citrate, sodium gluconate, potassium tartrate, potassium citrate, potassium gluconate, ammonium tartrate, ammonium malate, ammonium citrate, ammonium gluconate, monoethanolamine, triethylenetetramine and tetraethylenepentamine.
2. The high current density resistant acidic zinc-nickel electroplating bath as claimed in claim 1, wherein: the conductive salt is at least one of potassium chloride, sodium chloride, potassium sulfate and sodium sulfate.
3. The high current density resistant acidic zinc-nickel electroplating bath as claimed in claim 1, wherein: the pH buffering agent is at least one of boric acid, borate, acetic acid, acetate, citric acid and citrate.
4. The high current density resistant acidic zinc-nickel electroplating bath as claimed in claim 1, wherein: the brightener is at least one of benzalacetone, dibenzylidene acetone, aromatic acetone, methyl naphthylethanone, methyl naphthylacetone, o-chlorocinnamic acid, o-chlorobenzaldehyde, cinnamic acid, coumarin, polyethylene glycol and triethanolamine.
5. A method for electroplating zinc and nickel is characterized in that: a substrate is plated with the high current density resistant acidic zinc-nickel plating solution according to any one of claims 1 to 4.
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| CN109609979B (en) * | 2019-02-19 | 2020-01-14 | 广州睿邦新材料科技有限公司 | Multi-layer nickel electroplating additive for improving stability |
| CN112481667B (en) * | 2020-11-03 | 2021-12-07 | 深圳市恒兴安实业有限公司 | Zinc-nickel alloy electroplating process |
| CN114525555B (en) * | 2022-02-22 | 2023-12-01 | 太仓鑫天健环保科技有限公司 | Acidic zinc-nickel alloy electroplating additive and electroplating solution |
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| CN105102689A (en) * | 2013-03-27 | 2015-11-25 | 日本表面化学株式会社 | Zinc-nickel alloy plating solution and plating method |
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| JPH01219188A (en) * | 1988-02-26 | 1989-09-01 | Okuno Seiyaku Kogyo Kk | Zinc-nickel alloy plating bath |
| JP4447100B2 (en) * | 2000-02-15 | 2010-04-07 | ディップソール株式会社 | Alkaline zinc and zinc alloy plating bath |
| US20050133376A1 (en) * | 2003-12-19 | 2005-06-23 | Opaskar Vincent C. | Alkaline zinc-nickel alloy plating compositions, processes and articles therefrom |
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| CN105102689A (en) * | 2013-03-27 | 2015-11-25 | 日本表面化学株式会社 | Zinc-nickel alloy plating solution and plating method |
| CN106661750A (en) * | 2014-10-27 | 2017-05-10 | 安美特德国有限公司 | Acidic zinc and zinc nickel alloy plating bath composition and electroplating method |
| CN106011953A (en) * | 2016-06-12 | 2016-10-12 | 南通创源电化学科技有限公司 | Acid zinc-nickel alloy electroplating process applied to automobile parts |
| CN106435670A (en) * | 2016-11-29 | 2017-02-22 | 江苏澳光电子有限公司 | Zinc-nickel alloy plating liquid and application thereof |
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