CN115787001A - High-corrosion-resistance white chromium electroplating solution and electroplating process using same - Google Patents
High-corrosion-resistance white chromium electroplating solution and electroplating process using same Download PDFInfo
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Abstract
The invention relates to the technical field of metal plating, and discloses a high-corrosion-resistance white chromium electroplating solution and an electroplating process using the same, wherein the white chromium electroplating solution comprises the following raw materials in percentage by mass: 10-15g/L of trivalent chromium ions, 26-33g/L of complexing agent sodium formate dihydrate, 25-32g/L of ammonium sulfate, 70-80g/L of potassium sulfate and 110-130g/L of sodium sulfate; trivalent chromium ions in the electroplating solution provide metal chromium for the electroplating layer, and the ammonium sulfate conductive salt can adjust the conductivity of the electroplating solution, improve the covering performance and the thickness of the electroplating layer and meet the test requirement on corrosion resistance; according to the electroplating process using the high-corrosion-resistance white chromium electroplating solution, sulfate electroplating solution containing ammonium sulfate is used, and the prepared plating layer is a blue-white-luster chromium plating layer which is of a microcrack structure and has high corrosion resistance under the conditions that the temperature is 30-40 ℃ and the pH value is 3.0-3.5.
Description
Technical Field
The invention relates to the technical field of metal electroplating, in particular to a high-corrosion-resistance white chromium electroplating solution and an electroplating process using the same.
Background
The electroplated white chromium coating not only has good color, but also has higher corrosion resistance.
The prior art trivalent chromium electroplating process uses chromium plating solution systems to include chloride solution systems and sulfate solution systems. The chloride solution system uses chromium chloride as main salt, the anode has good conductivity, the cost is low, the electrodeposition speed is high, and the cathode current efficiency is high; however, the precipitated chlorine generates strong corrosion to equipment, and the obtained chromium plating layer is whitish in appearance, mostly has a microporous structure and is poor in corrosion resistance. Chromium sulfate is used as a main salt in a sulfate solution system, so that the defects of poor dispersing capacity and covering capacity of a plating solution exist, the thickness of the prepared plating layer is insufficient, and the defects of scorching and plating leakage of the plating layer are easy to occur; the quality requirement of 85-hour corrosion resistance detection of the acetate fog test (AASS) of GB/T10125-1997 standard of a client cannot be met.
Disclosure of Invention
In view of the above problems, a first objective of the present invention is to provide a white chromium electroplating solution with high corrosion resistance, which adopts a sulfate solution system, has good coverage performance and plating thickness, and can meet the quality requirement of corrosion resistance detection.
The invention also aims to provide an electroplating process using the white chromium electroplating solution with high corrosion resistance to prepare a white chromium coating with a microcrack structure and better corrosion resistance.
In order to achieve the purpose, the invention adopts the following technical scheme:
a high-corrosion-resistance white chromium electroplating solution comprises the following raw materials in percentage by mass: 10-15g/L of trivalent chromium ions, 26-33g/L of complexing agent sodium formate dihydrate, 25-32g/L of ammonium sulfate, 70-80g/L of potassium sulfate and 110-130g/L of sodium sulfate;
the trivalent chromium ions are obtained by dissolving chromium sulfate in pure water.
Furthermore, the raw material also comprises 0.01-0.02g/L of surfactant sodium dodecyl sulfate according to the mass concentration.
Furthermore, the raw material also comprises 10-15g/L of auxiliary complexing agent glycine according to the mass concentration.
Furthermore, the raw material also comprises 60-65g/L of boric acid serving as a buffering agent according to the mass concentration.
Furthermore, the raw material also comprises an additive SH 4-8mL/L according to the mass concentration.
Preferably, the pH is 3.0 to 3.5.
Further, the invention provides a white chromium electroplating process for metal parts, which uses the white chromium electroplating solution with high corrosion resistance, and comprises the following steps:
(1) Weighing the components of the electroplating solution according to a formula, and preparing the high-corrosion-resistance white chromium electroplating solution;
(2) The method comprises the steps of taking a metal piece as a cathode, carrying out pretreatment of oil removal, acid washing, alkali washing and activation on the cathode, placing an anode and the pretreated cathode into the high-corrosion-resistance white chromium electroplating solution in an electroplating bath, controlling the temperature of the high-corrosion-resistance white chromium electroplating solution to be 30-40 ℃ and the pH value to be 3.0-3.5, and introducing current for electroplating under a stirring state for 2-4min.
Preferably, cu is in the plating bath 2+ 、Zn 2+ 、Ni 2+ 、Fe 2+ The content of (b) is not more than 25mg/L, 40mg/L, 170mg/L and 64mg/L respectively.
Preferably, the current density is 10-14A/dm 2 。
Preferably, the anode is a titanium-based coated iridium oxide anode or a graphite anode.
The technical scheme of the invention has the beneficial effects that: the high-corrosion-resistance white chromium electroplating solution is a sulfate system, trivalent chromium ions in the electroplating solution provide metal chromium for an electroplated layer, and ammonium sulfate conductive salt is introduced to adjust the conductivity of the electroplating solution, so that the high-corrosion-resistance white chromium electroplating solution has good covering performance and coating thickness, and can meet the 85-hour corrosion resistance requirement of an acetate fog test (AASS) in GB/T10125-1997 standard.
Furthermore, the electroplating process using the white chromium electroplating solution with high corrosion resistance provided by the invention uses a sulfate electroplating solution containing ammonium sulfate, and under the conditions of 30-40 ℃ and pH value of 3.0-3.5, the prepared white chromium plating layer is of a microcrack structure and has better corrosion resistance.
Drawings
FIG. 1 is a SEM micrograph of example 1 of the present invention;
FIG. 2 is a SEM micrograph of comparative example 1 of the present invention;
FIG. 3 is a SEM micrograph of comparative example 2 of the present invention;
FIG. 4 is a SEM micrograph of comparative example 3 of the present invention;
FIG. 5 is a SEM micrograph of comparative example 4 of the present invention;
FIG. 6 is a SEM micrograph of comparative example 5 of the present invention;
FIG. 7 is a SEM micrograph of comparative example 6 of the present invention;
fig. 8 is a SEM micrograph of comparative example 7 of the present invention.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
In the description herein, references to the description of the terms "embodiment," "example," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
A high-corrosion-resistance white chromium electroplating solution comprises the following raw materials in percentage by mass: 10-15g/L of trivalent chromium ions, 26-33g/L of complexing agent sodium formate dihydrate, 25-32g/L of ammonium sulfate, 70-80g/L of potassium sulfate and 110-130g/L of sodium sulfate;
the trivalent chromium ions are obtained by dissolving chromium sulfate in pure water.
The high-corrosion-resistance white chromium electroplating solution is a sulfate system, trivalent chromium ions in the electroplating solution provide metal chromium for an electroplated layer, and ammonium sulfate conductive salt is introduced to adjust the conductivity of the electroplating solution, so that the high-corrosion-resistance white chromium electroplating solution has good covering performance and coating thickness, and can meet the 85-hour corrosion resistance requirement of an acetate fog test (AASS) of QB10125-1997 standard.
When Cr is contained in the plating solution 3+ When the concentration is increased, the thickness of the obtained coating is also gradually increased, and the change of the coverage range of the coating is firstly increased and then decreased; when Cr is present 3+ If the concentration exceeds 15g/L, free [ Cr (H) exists in the plating liquid 2 O) 6 ] 3+ The crystal grains of the metal chromium precipitated during electrodeposition are enlarged, and the coating is easy to have the defect of scorching or peeling; when Cr is present 3+ When the concentration is less than 10g/L, the content of the generated active complex is low, the electrodeposition speed is slow, the thickness of the coating is thin, and the quality requirement of corrosion resistance is difficult to meet.
The addition of conductive ammonium sulfate can increase the conductivity of the electroplating solution, thereby being beneficial to energy conservation; the added ammonium sulfate can improve the plating leakage defect of a high current density area and can also avoid the phenomenon of scorching of a plating layer; when the concentration of the ammonium sulfate as a conductive salt exceeds 32g/L, the potential of the plating solution is lowered too much, resulting in a thin plating layer which does not satisfy the quality requirements.
The sodium sulfate and the potassium sulfate in the formula are both used for enhancing the conductivity of the electroplating solution, and the conductivity of the electroplating solution is not increased much by the ammonium sulfate with the concentration of 25-32g/L, so that the sodium sulfate and the potassium sulfate need to be supplemented to increase the conductivity of the electroplating solution, and the sodium sulfate and the potassium sulfate have the advantage of low cost.
[Cr(H 2 O) 6 ] 3+ With regular octahedral structure, the electrochemical activity is relatively low, if free [ Cr (H) is present in the plating bath 2 O) 6 ] 3+ And the electrodeposition reaction is difficult to occur at the cathode to generate an acceptable chromium plating layer.
Sodium formate dihydrate, HCOO, as an added complexing agent - Can be free from Cr (H) in the plating solution 2 O) 6 ] 3+ Complexing to formElectrochemically active [ Cr (H) 2 O) 5 (HCOO) 2 ] 2+ Complex ions, so that the speed of the electrodeposition reaction can be improved; however, when the concentration of the sodium diformate reaches 36g/L, the coverage range of the plating layer is narrowed, and a severe plating leakage phenomenon can occur in a low current density area.
Furthermore, the raw material also comprises 0.01-0.02g/L of surfactant sodium dodecyl sulfate according to the mass concentration.
And a proper amount of sodium dodecyl sulfate is added to be used as a surfactant, so that the surface wettability of an electroplated workpiece can be improved, and the adhesive force of a plating layer can be improved.
Furthermore, the raw material also comprises 10-15g/L of auxiliary complexing agent glycine according to the mass concentration.
The glycine is beneficial to increasing the stability of the electroplating solution, so that the quality of the plating layer is improved, the coverage area of the plating layer is increased along with the increase of the concentration of the glycine serving as an auxiliary complexing agent, but the thickness of the plating layer is gradually reduced. The concentration of the auxiliary complexing agent glycine is controlled to be 10-15g/L, so that the thickness of the plating layer can be kept above 0.50 mu m, and a better coverage range of the plating layer is kept.
Further, the raw material also comprises 60-65g/L of boric acid serving as a buffering agent according to the mass concentration.
Boric acid is pH buffer and can complex hydroxide ions in water molecules to release H + To replenish H consumed by hydrogen evolution reaction in the electroplating process + Thereby stabilizing the pH of the plating solution.
When the concentration of boric acid is less than 60g/L, the coverage range of the plating layer is narrow; when the boric acid concentration is more than 65g/L, the boric acid may be precipitated in the form of crystals, which may affect the dissolution of the conductive salt in the plating solution, resulting in a decrease in the conductive ability of the plating solution.
Furthermore, the raw material also comprises additive SH 4-8mL/L according to the mass concentration.
Sulfur-containing additives SN, WS, SH and TS, and an organic amine additive TH can improve the dispersing capacity and covering capacity of the electroplating solution, so that the improvement of cathode current efficiency and the increase of the thickness of the plating layer are facilitated, the appearance and the color of the obtained plating layer are different, and the appearance effect of the plating layer only added with SH meets the appearance requirement of the white chromium plating layer.
Preferably, the pH is 3.0 to 3.5.
Taking a Hull cell experiment with the temperature of 30 ℃, the current of 5A and the electroplating time of 3min as an example, when the pH value of the electrolyte is 1.5, the displacement of the plating layer is extremely poor, the thickness of the formed plating layer is less than 0.3 μm, and the coverage range of the plating layer is only 2.3cm; with the increase of the pH value of the electrolyte, the thickness of the plating layer and the covering capacity of the electroplating solution are correspondingly increased; when the pH value is 3.0, the thickness of the plating layer can exceed 0.5 mu m, and the coverage range of the plating layer is 6.8cm; when the pH value is 3.5, the thickness of the plating layer is 0.3 mu m, and the optimal coverage range of the plating layer can reach 7.9cm; therefore, the pH of the plating solution is preferably selected to be 3.0 to 3.5.
Further, the invention provides a white chromium electroplating process for metal parts, which uses the white chromium electroplating solution with high corrosion resistance, and comprises the following steps:
(1) Weighing the components of the electroplating solution according to a formula, and preparing the high-corrosion-resistance white chromium electroplating solution;
(2) The method comprises the steps of taking a metal piece as a cathode, carrying out pretreatment of oil removal, acid washing, alkali washing and activation on the cathode, placing an anode and the pretreated cathode into the high-corrosion-resistance white chromium electroplating solution in an electroplating bath, controlling the temperature of the high-corrosion-resistance white chromium electroplating solution to be 30-40 ℃ and the pH value to be 3.0-3.5, and introducing current for electroplating under a stirring state for 2-4min.
The white chromium electroplating process for the metal piece uses sulfate electroplating solution containing ammonium sulfate to prepare a chromium plating layer with the thickness of 0.45-0.67 mu m and the color of white slightly blue light under the conditions of 30-40 ℃ and the pH value of 3.0-3.5, wherein the plating layer is of a microcrack structure and has better corrosion resistance.
When the temperature is 25 ℃, the covering capacity of the coating can reach the optimal state, but the thickness of the coating is only 0.36 μm; when the temperature reaches 45 ℃, the covering capability of the plating layer is insufficient, and the phenomenon of plating leakage is easy to occur.
Preferably, cu is in the plating bath 2+ 、Zn 2+ 、Ni 2+ 、Fe 2+ The content of (b) is not more than 25mg/L, 40mg/L, 170mg/L and 64mg/L respectively.
The Cu in the electroplating solution can be effectively reduced by cleaning the cylinder periodically and adopting low-current electrolysis before electroplating the workpiece 2+ 、Zn 2+ 、Ni 2+ And Fe 2+ The content of the metal impurities in the trivalent chromium plating solution can effectively prevent the influence of the metal impurities on the color of the trivalent chromium plating layer, thereby improving the electroplating quality of the product.
Preferably, the current density is 10-14A/dm 2 。
When the current density is 8A/dm 2 When the electroplating solution is used, the thickness of the electroplating layer is thin, and the phenomenon of plating leakage occurs; the current density is increased from low to high when the current density is 10A/dm 2 When the coating is used, the coating is uniform and bright, and the thickness of the coating reaches the maximum value; continuously increasing the current density, gradually decreasing the thickness of the coating, and when the current density is more than 14A/dm 2 In the case of this, the thickness of the plating layer is less than 0.5. Mu.m.
Preferably, the anode is a titanium-based coated iridium oxide anode or a graphite anode.
The titanium-based coating iridium oxide anode, commonly called DSA anode, has smaller oxygen evolution overpotential, can inhibit the generation of hexavalent chromium, ensures that trivalent chromium in the electroplating solution is not easily oxidized, and has the advantage of longer service life.
The graphite anode has the advantages of low price, corrosion resistance, good conductivity, higher current efficiency, better covering capacity and the like, but the graphite anode cannot inhibit the generation of hexavalent chromium in the electroplating solution.
Example 1 and comparative examples 1 to 7
1. Each example and each comparative example were prepared by placing the plating solutions in accordance with the raw materials listed in Table 1, conducting the plating experiment using a square bath having a volume of 560mL and a size of 11.0 cm. Times.6.0 cm. Times.8.5 cm, to which the plating solution was added in a volume of 250mL, using a bright nickel plated brass sheet of 6.0 cm. Times.5.0 cm as the cathode and a titanium-based coated iridium oxide anode, to prepare three test pieces for each example and each comparative example.
2. The AASS acetate spray test was conducted according to the regulations of GB/T10125-1997 on each of the examples and each of the three test pieces in each comparative example, and the time and the average value of red rust development were recorded and calculated for each of the examples and each of the three test pieces in each comparative example, and the test results are shown in Table 2.
3. The thickness of the plating layer of each example and three test pieces of each comparative example was measured using an X-ray fluorescence thickness gauge, and the average value thereof was calculated, and the test results are shown in table 2.
4. The surface morphology of the plating layer of each example and each comparative test piece was observed using a scanning electron microscope.
5. The bonding force of the plating layers of the test sample pieces of each example and each comparative example was tested by a bending test method and a scribing and ruling test method, and the test results are shown in table 2:
1) Bending test: the test piece is rapidly and repeatedly bent by 180 degrees by using a pliers until the test piece is broken, and the plating layer is qualified without scraps or other peeling phenomena;
2) Scribing and grid drawing test: in the experiment, a hard steel scriber with a cutting edge of 30 degrees is selected, two parallel lines are scribed on the surface of the test piece at a distance of about 2mm, so that the hard steel scriber can scribe the substrate once, and the existence of any part of the plating layer between the two scribed lines is observed to be separated from the metal layer of the substrate.
TABLE 1 raw material composition and plating Process parameters of examples and comparative examples
TABLE 2 test results of examples and comparative examples
The data and test results of tables 1 and 2 above were analyzed and are summarized as follows:
1. the coating of the embodiment 1 is white and slightly blue, and as can be seen from the electronic scanning picture shown in the attached drawing 1, the appearance of the coating is a microcrack result, the thickness of the coating reaches 0.81 μm, and the occurrence time of rusty spots in an AASS (anti-corrosion performance) test is 90 hours; the plating solution of comparative example 1 is different from that of example 1 in that ammonium sulfate is not added, and as shown in the electronic scanning picture of fig. 2, the rust-spot occurrence time of the corrosion resistance test of the AASS test of comparative example 1 is 82h; the plating solution of comparative example 7 was a hexavalent chromium plating solution, and the rust-spot occurrence time of the corrosion resistance test of the AASS test of comparative example 7 was 68 hours, as shown in the electronic scanning picture of fig. 8; the corrosion resistance of example 1 is better than that of comparative example 7 and comparative example 1.
2. The differences of comparative example 2 compared to example 1 are: comparative example 2 does not use the additive SH, and the color of the plating layer of comparative example 2 is dark and bright, and as shown in the electronic scanning picture of FIG. 3, the rusty spot appearance time of the corrosion resistance test of AASS test is 59h, which can not meet the requirement.
3. The differences of comparative example 3 compared to example 1 are: the additive used in the comparative example 3 is SN, the color of the plating layer of the comparative example 3 is blue and white, and as shown in an electronic scanning picture of FIG. 4, the rusty spot occurrence time of the corrosion resistance test of the AASS test is 47h, and the corrosion resistance performance is not satisfactory.
4. The differences of comparative example 4 compared to example 1 are: the additive used in the comparative example 4 is TH, the color of the plating layer of the comparative example 4 is black and bright, and as shown in an electronic scanning picture of FIG. 5, the rusty spot occurrence time of the corrosion resistance test of the AASS test is 69h, and the corrosion resistance performance does not meet the requirement.
5. The differences of comparative example 5 compared to example 1 are: the additive used in comparative example 5 was WS, and the color of the plating layer of comparative example 5 was clear black, and as shown in the electronic scanning picture of fig. 6, the occurrence time of rust in the corrosion resistance test of AASS test was 159 hours, and the color of the plating layer did not meet the requirements in spite of the energy consumption for corrosion resistance.
6. The differences of comparative example 6 compared to example 1 are: the additive used in the comparative example 6 is TS, the color of the plating layer of the comparative example 6 is blue and white, and as shown in an electronic scanning picture of FIG. 7, the rust occurrence time of the corrosion resistance test of the AASS test is 57h, and the corrosion resistance performance is not satisfactory.
In conclusion, the white chromium electroplating solution with high corrosion resistance is a sulfate system, trivalent chromium ions in the electroplating solution provide metal chromium for an electroplated layer, and ammonium sulfate conductive salt is introduced to adjust the conductivity of the electroplating solution, so that the white chromium electroplating solution has good covering performance and coating thickness, and can meet the requirement of 85-hour corrosion resistance of an acetate fog test (AASS) in GB/T10125-1997 standard.
Furthermore, the electroplating process using the white chromium electroplating solution with high corrosion resistance provided by the invention uses sulfate electroplating solution containing ammonium sulfate, and the prepared white chromium plating layer is of a micro-crack structure and has better corrosion resistance under the conditions of 30-40 ℃ and pH value of 3.0-3.5.
The technical principle of the present invention is described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without inventive effort, which would fall within the scope of the present invention.
Claims (10)
1. The high-corrosion-resistance white chromium electroplating solution is characterized by comprising the following raw materials in percentage by mass: 10-15g/L of trivalent chromium ions, 26-33g/L of complexing agent sodium formate dihydrate, 25-32g/L of ammonium sulfate, 70-80g/L of potassium sulfate and 110-130g/L of sodium sulfate;
the trivalent chromium ions are obtained by dissolving chromium sulfate in pure water.
2. The highly corrosion-resistant white chromium electroplating bath according to claim 1, wherein the raw material further comprises 0.01-0.02g/L of sodium lauryl sulfate as a surfactant, calculated by mass concentration.
3. The white chromium electroplating bath with high corrosion resistance according to claim 1, wherein the raw material further comprises 10-15g/L of glycine as an auxiliary complexing agent, calculated according to mass concentration.
4. The white chromium electroplating bath with high corrosion resistance according to claim 1, wherein the raw material further comprises boric acid as a buffer in an amount of 60 to 65g/L in terms of mass concentration.
5. The white chromium electroplating bath having high corrosion resistance according to claim 1, wherein the raw material further comprises an additive SH 4-8mL/L in terms of mass concentration.
6. The highly corrosion-resistant white chromium electroplating bath according to claim 1, wherein the pH is 3.0 to 3.5.
7. A white chromium electroplating process for metal parts, characterized in that the white chromium electroplating solution with high corrosion resistance of any one of claims 1 to 6 is used, and comprises the following steps:
(1) Weighing the components of the electroplating solution according to a formula, and preparing the high-corrosion-resistance white chromium electroplating solution;
(2) The method comprises the steps of taking a metal piece as a cathode, carrying out pretreatment of oil removal, acid washing, alkali washing and activation on the cathode, placing an anode and the pretreated cathode into the high-corrosion-resistance white chromium electroplating solution in an electroplating bath, controlling the temperature of the high-corrosion-resistance white chromium electroplating solution to be 30-40 ℃ and the pH value to be 3.0-3.5, and introducing current for electroplating under a stirring state for 2-4min.
8. White chrome plating process for metal parts as claimed in claim 7, characterized in that Cu is in the plating bath 2+ 、Zn 2+ 、Ni 2+ 、Fe 2+ The content of (b) is not more than 25mg/L, 40mg/L, 170mg/L and 64mg/L respectively.
9. The white chromium electroplating process for metal parts according to claim 7, characterized in that the current density is 10-14A/dm 2 。
10. The white chromium electroplating process for metal parts according to claim 7, characterized in that the anode is a titanium-based coated iridium oxide anode or a graphite anode.
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| RU2814771C1 (en) * | 2023-08-31 | 2024-03-04 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Российский химико-технологический университет имени Д.И. Менделеева" (РХТУ им. Д.И. Менделеева) | Method of electroplating chromium coatings from electrolyte based on hexahydrate of chromium (iii) sulphate and sodium formate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| RU2814771C1 (en) * | 2023-08-31 | 2024-03-04 | Федеральное государственное бюджетное образовательное учреждение высшего образования "Российский химико-технологический университет имени Д.И. Менделеева" (РХТУ им. Д.И. Менделеева) | Method of electroplating chromium coatings from electrolyte based on hexahydrate of chromium (iii) sulphate and sodium formate |
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