CN112517859B - Environment-friendly anti-discoloration corrosion-resistant tin plating preparation process for chaplet - Google Patents
Environment-friendly anti-discoloration corrosion-resistant tin plating preparation process for chaplet Download PDFInfo
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- CN112517859B CN112517859B CN202011326421.5A CN202011326421A CN112517859B CN 112517859 B CN112517859 B CN 112517859B CN 202011326421 A CN202011326421 A CN 202011326421A CN 112517859 B CN112517859 B CN 112517859B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22C—FOUNDRY MOULDING
- B22C21/00—Flasks; Accessories therefor
- B22C21/12—Accessories
- B22C21/14—Accessories for reinforcing or securing moulding materials or cores, e.g. gaggers, chaplets, pins, bars
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- C—CHEMISTRY; METALLURGY
- 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
- C25D3/30—Electroplating: Baths therefor from solutions of tin
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/10—Electroplating with more than one layer of the same or of different metals
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
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Abstract
An environment-friendly discoloration-resistant corrosion-resistant tinning preparation process for a chaplet comprises the following steps: (1) pretreatment: sequentially carrying out pretreatment of chemical oil removal, acid pickling rust removal and activation on the chaplet; (2) electroplating tin: placing the pretreated chaplet in a first electroplating bath, wherein the electroplating bath comprises an electroplating bath, a constant current/constant potential instrument, an anode, an electroplating bath heating device, a temperature sensor, a height adjusting block and a lifting device; the first plating solution comprises stannous methanesulfonate stock solution, methanesulfonic acid, an additive, 2, 5-dihydroxybenzenesulfonate and deionized water; (3) cleaning; (4) electroplating tin; (5) cleaning; (6) anti-discoloration treatment; (7) and (5) drying. The environment-friendly anti-tarnishing and corrosion-resistant tinning preparation process for the chaplet, disclosed by the invention, has the advantages of reasonable and simple process steps and strong operability, and solves the technical problems of great environmental pollution, poor corrosion-resistant effect and poor tarnishing-resistant effect of a tinning layer in the chaplet tinning preparation process in the prior art.
Description
Technical Field
The invention belongs to the technical field of chaplet preparation, and particularly relates to an environment-friendly anti-tarnishing and corrosion-resistant tinning preparation process for chaplets.
Background
The core support is a metal support for supporting the core in the casting mold, and the material of the core support is the same as or close to that of the casting. For rust protection and better fusion with molten metal, the chaplet surface should be cleaned and tin plated. Tin is a metal with better plasticity, is very convenient to roll, punch and stretch, is easy to brush, polish or heat to melt into a finished product, has good corrosion resistance, environmental protection, solderability, flexibility, ductility and the like, is not easy to lose luster, has high chemical stability, does not generate chemical reaction in the air at normal temperature, is stable in fresh water or seawater, and is not easy to corrode in the presence of halogen, mineral acid and strong alkaline solution.
With the continuous development of economy, the development speed of the industry of the cast finished products is higher, the demand of the cast finished products on the chaplet is relatively higher, and the quality requirement on the chaplet is relatively higher. The tin plating process is one of core processes of the core support, and the quality of the tin plating process plays an important role in the quality of the core support and a cast finished product. The currently used tin plating processes mainly comprise five types, including sulfate tin plating, halide tin plating, fluoboric acid tin plating and alkaline tin plating, and all the five tin plating processes have certain defects, such as no deoiling capability of sulfate in the sulfate tin plating and strict requirements on pretreatment of electroplating; the halogen tin electroplating belongs to a normal-temperature tinning process, sludge is easy to generate, more than 20% of tin enters the sludge, the sludge is difficult to treat and the cost is high, and a fluoride is added into a plating solution, so that certain pollution is caused to the environment; the borate tinning has a wider current density range, higher electrodeposition speed and dispersion capacity, bright, crystalline, fine and compact plating layer and the defects of higher corrosivity, toxicity and cost; stannate tin plating has large energy consumption, narrow current density range, low current efficiency and large influence on anode behavior, and a bright coating cannot be directly obtained.
Therefore, a preparation process of the environment-friendly, tarnish-resistant and corrosion-resistant tin plating suitable for the chaplet needs to be developed, and the preparation process has high added value and wide application prospect.
Chinese patent application No. CN201910994659.6 discloses a method for plating tin on a metal surface, which is to contact a non-plated tin portion with a repair solution to perform a chemical reaction, so as to achieve rapid tin plating without further improving the environmental protection, discoloration resistance and corrosion resistance of tin plating.
Disclosure of Invention
The invention aims to: in order to overcome the defects, the invention aims to provide the environment-friendly anti-tarnishing and anti-corrosion tin plating preparation process for the chaplet, which has reasonable and simple process steps and strong operability, solves the technical problems of larger environmental pollution, poor corrosion resistance effect of a tin plating layer and poor tarnishing resistance effect in the chaplet tin plating preparation process in the prior art, greatly improves the corrosion resistance and the tarnishing resistance of the chaplet through secondary tin plating and tarnishing resistance treatment, and has wide application prospect.
The purpose of the invention is realized by the following technical scheme:
an environment-friendly discoloration-resistant corrosion-resistant tinning preparation process for a chaplet comprises the following steps:
(1) pretreatment: sequentially carrying out pretreatment of chemical oil removal, acid pickling rust removal and activation on the chaplet;
(2) Electroplating tin: placing the pretreated chaplet in a first electroplating bath, wherein the electroplating bath comprises an electroplating bath, a constant current/constant potential instrument, an anode, an electroplating bath heating device, a temperature sensor, a height adjusting block and a lifting device; a first plating solution is contained in the plating bath, the pretreated chaplet is used as a cathode and is vertically arranged in the plating bath in parallel with an anode, and the anode is a titanium coating anode plate; the anode is connected with the anode of the constant current/constant potential instrument through an anode line, and the pretreated chaplet is connected with the cathode of the constant current/constant potential instrument through a cathode line; the plating bath heating device is a snakelike titanium alloy heating pipe, and the snakelike titanium alloy heating pipe is arranged in the plating bath for heating; a temperature sensor is arranged in the plating bath; the height adjusting block is arranged in the electroplating bath and is connected with a lifting device positioned outside the electroplating bath, and the volume of the height adjusting block immersed in the first plating solution is adjusted through the lifting device, so that the control of the height of the tin liquid level is realized; the first plating solution comprises stannous methanesulfonate stock solution, methanesulfonic acid, an additive, 2, 5-dihydroxybenzenesulfonate and deionized water; the thickness of the tin coating is 0.5-1 μm;
(3) Cleaning: washing and drying the electroplated chaplet;
(4) electroplating tin: placing the chaplet into a second electroplating bath, wherein a second plating solution is contained in the second electroplating bath; the structure of the second electroplating bath is the same as that of the first electroplating bath; the second plating solution comprises tin alkyl sulfonate, alkyl sulfonic acid, a wetting agent, a brightening agent, a stabilizing agent and deionized water; the thickness of the tin coating is 2-4 μm;
(5) cleaning: washing and drying the electroplated chaplet;
(6) anti-discoloration treatment: placing the chaplet in a treatment tank, soaking for 2-5min at 45-55 ℃, wherein the treatment tank is filled with anti-tarnishing treatment liquid; the anti-tarnishing treatment liquid comprises phosphoric acid, organic composite acid, a corrosion inhibitor, an additive and deionized water;
(7) drying: and drying the chaplet.
The environment-friendly anti-tarnishing and corrosion-resistant tin plating preparation process for the chaplet, disclosed by the invention, has the advantages of reasonable and simple process steps and strong operability, solves the technical problems of great environmental pollution, poor corrosion resistance effect and poor tarnishing resistance effect of a tin plating layer in the traditional chaplet tin plating preparation process, and greatly improves the corrosion resistance and the tarnishing resistance of the chaplet through secondary tin plating and tarnishing resistance treatment.
Wherein, the first plating solution and the second plating solution both adopt stannous methanesulfonate stock solution, methanesulfonic acid, alkyl tin sulfonate, alkyl sulfonic acid and other sulfonates, the biodegradability is better, the toxicity of the degraded micromolecule is much lower, and the degraded micromolecule does not have negative influence or has little influence on the environment after degradation treatment; 2, 5-dihydroxybenzenesulfonate is used as an antioxidant in the first plating solution, so that the first plating solution has good biodegradability, and can not cause negative effects or have little effects on the environment after degradation treatment; the anti-tarnishing treatment fluid, the phosphoric acid and the organic composite acid have the effects of slightly dissolving local crystal grain bulges of the tin plating, the composite corrosion inhibitor has the effect of forming a chemical adsorption film on the surface of a tin plating layer under the action of the acid, the additive has the effect of improving the stability and the anti-tarnishing capacity of the tin plating surface in high-temperature and high-humidity environments, does not contain chromium, heavy metal ions and other harmful components, is an environment-friendly aqueous solution, is simple to operate, and can form a thin, transparent and compact anti-tarnishing protection film on the surface of the core support tin plating by soaking for 2-5min at the temperature of 45-55 ℃.
Further, the pretreatment of the environment-friendly discoloration-resistant corrosion-resistant tin plating preparation process for the chaplet specifically comprises the following steps:
(1) Chemical oil removal: cleaning the surface of the core support by adopting deoiling liquid, and washing the surface of the core support by using clear water; the deoiling liquid is prepared from NaOH and Na2CO3、Na3PO4·12H2O、Na2SiO3·9H2O and deionized water;
(2) acid pickling for rust removal: pickling the surface of the chaplet by using dilute sulfuric acid with the volume fraction of 5% at room temperature, and washing the surface of the chaplet by using clear water;
(3) activation: and activating the chaplet by adopting a methanesulfonic acid solution.
In order to improve the effect of the electrolytic tinning, the core support is firstly pretreated by chemical oil removal, acid pickling rust removal and activation. The core support is usually polluted by oil in the processing process, and the polluted part can not contact with plating solution, so that the part generates plating leakage, and sometimes oil stains can also cause the bubbling, falling and the like of a plating layer; the surface of the chaplet is pickled by dilute sulphuric acid with volume fraction of 5% at room temperature to remove surface impurities, and simultaneously, the micro roughness can be increased, and the binding force between a plating layer and the chaplet surface is improved; the aim of activation is to react with the surface of the chaplet to enable the metal crystal to be in an activated state, thus not only ensuring the bonding force of the plating layer and the chaplet, but also preventing the chaplet from secondary oxidation. In order to avoid contamination of the bath with other activating acid solutions, acids other than methanesulfonic acid cannot be used in the activation.
Further, in the environment-friendly anti-tarnishing and corrosion-resistant tin plating preparation process for the chaplet, the dosage of NaOH in the deoiling liquid is 60-80 g.L-1，Na2CO3The dosage of the composition is 20-30 g.L-1，Na3PO4·12H2The dosage of O is 30-40 g.L-1，Na2SiO3·9H2The dosage of O is 5-10 g.L-1。
Furthermore, in the preparation process of the environment-friendly anti-tarnishing and corrosion-resistant tinning for the chaplet, the consumption of the stannous methanesulfonate stock solution in the first tinning solution is 20-22 g.L-1The dosage of the methanesulfonic acid is 40-45 ml.L-1The dosage of the additive is 4-5 ml.L-1The dosage of the antioxidant is 15-20 ml.L-1(ii) a The electrotinning current density of the step (2) is 1-1.5 A.dm-2The electroplating time is 1-2 min, and the temperature is 40-50 ℃.
Further, in the environment-friendly anti-tarnishing and corrosion-resistant tin plating preparation process for the chaplet, the dosage of the tin alkyl sulfonate in the plating solution II is 45-50 g.L-1The dosage of the alkyl sulfonic acid is 120-140 ml.L-1The dosage of the wetting agent is 50-70 ml.L-1The amount of brightener is 3-5 ml.L-1The dosage of the stabilizer is 2-4 ml.L-1(ii) a The current density of the electrotinning in the step (4) is 1-1.5 A.dm-2The electroplating time is 1-2 min, and the temperature is 55-60 ℃.
Furthermore, in the environment-friendly anti-tarnishing and corrosion-resistant tinning preparation process for the chaplet, the dosage of phosphoric acid in the anti-tarnishing treatment liquid is 10-15 g.L -1The dosage of the organic composite acid is 30-35 g.L-1The dosage of the corrosion inhibitor is 0.1-0.5 g.L-1, the dosage of the additive is 0.1-0.2 g.L-1。
Further, in the environment-friendly anti-tarnishing and corrosion-resistant tin plating preparation process for the chaplet, the temperature sensor comprises a deep groove zone thermocouple and a shallow groove zone thermocouple, the deep groove zone thermocouple is arranged at the bottom in the plating bath, and the shallow groove zone thermocouple is arranged at the upper part in the plating bath.
Because the temperature difference exists when the core support is arranged at the deep groove part and the shallow groove part of the electroplating bath in the working state of the electroplating bath, the temperature can be quickly adjusted according to the temperature change of tin liquid by arranging the deep groove area thermocouple and the shallow groove area thermocouple, and the precision of a temperature control system can be improved.
Furthermore, in the environment-friendly anti-tarnishing and corrosion-resistant tin plating preparation process for the chaplet, the first plating tank also comprises a control mechanism; the control mechanism comprises a PLC, an upper computer, a frequency converter and a PID controller, the PLC is in communication connection with the upper computer, the PLC receives and processes signals of the thermocouple in the deep groove area and the thermocouple in the shallow groove area, the PLC receives and processes signals of the constant current/constant potential rectifier and controls the constant current/constant potential rectifier, the PLC controls a lifting motor of the lifting device through the frequency converter, and the PLC controls the snakelike titanium alloy heating pipe through the PID controller.
The environment-friendly anti-tarnishing corrosion-resistant tin plating preparation process for the chaplet, disclosed by the invention, is high in intelligent degree, a PLC is used as a central processing unit, Siemens S7-300 and the like can be selected, and an upper computer monitors the temperature and constant current/constant potential instrument parameters obtained by the PLC on line by using a touch screen and can control the parameters through a human-computer interface of the upper computer. PLC passes through the converter and realizes the accurate control to elevator motor to the height of control altitude mixture control piece in the plating bath, when the altitude mixture control piece in the plating bath upwards or down moves, through the volume of adjusting the altitude mixture control piece in the immersion tin liquid, the realization is to the control of tin liquid level. The frequency converter can select Siemens general type frequency converter MicroMaster430, has high reliability and extreme flexibility, can switch between manual/automatic, very energy-conserving advantage. The frequency converter adopts an electromagnetic compatibility design, can quickly respond to acquired signals, but can well limit quick impact current so as to avoid influencing production due to an inadmissible tripping field in the operation of the machine.
The plating bath provided by the invention uses the snakelike titanium alloy heating pipe for heating, and the temperature signal acquired by the temperature sensor is sent to the PLC, the PLC controls the heating pipe in real time through the PID controller, so that the bath solution is heated, and the PID controller is adopted in the aspect of control.
Compared with the prior art, the invention has the following beneficial effects:
(1) the environment-friendly discoloration-resistant corrosion-resistant tin plating preparation process for the chaplet, disclosed by the invention, has the advantages of reasonable process steps, simplicity and strong operability, solves the technical problems of great environmental pollution, poor corrosion resistance effect and poor discoloration resistance effect of a tin plating layer in the chaplet tin plating preparation process in the prior art, greatly improves the corrosion resistance and discoloration resistance of the chaplet through secondary tin plating and discoloration resistance treatment, and has wide application prospect;
(2) according to the environment-friendly discoloration-resistant corrosion-resistant tin plating preparation process for the chaplet, stannous methanesulfonate stock solution, methanesulfonic acid, 2, 5-dihydroxybenzenesulfonate, alkyl tin sulfonate, alkyl sulfonic acid and other sulfonates are adopted in the first plating solution and the second plating solution, so that the biodegradation performance is good, the toxicity of degraded micromolecules is much lower, and no negative influence or little influence is caused on the environment after degradation treatment;
(3) according to the environment-friendly discoloration-resistant corrosion-resistant tin plating preparation process for the chaplet, the discoloration-resistant treatment liquid improves the stability and discoloration resistance of the tin plating surface in a high-temperature and high-humidity environment, does not contain harmful components such as chromium and heavy metal ions, is an environment-friendly aqueous solution, and is simple to operate;
(4) The environment-friendly discoloration-resistant corrosion-resistant tinning preparation process for the chaplet has high intelligent degree.
Drawings
FIG. 1 is a schematic structural diagram of a plating bath of the environmentally-friendly discoloration-resistant and corrosion-resistant tin plating preparation process for a chaplet according to the present invention;
FIG. 2 is a structural diagram of a control system of an electroplating bath of the environmentally-friendly discoloration and corrosion resistant tin plating preparation process for a chaplet according to the present invention;
in the figure: the device comprises a first electroplating bath 1, an electroplating bath 11, a constant current/constant potential instrument 12, an anode 13, an electroplating bath heating device 14, a temperature sensor 15, a deep groove area thermocouple 151, a shallow groove area thermocouple 152, a height adjusting block 16, a lifting device 17, a control mechanism 18, a PLC181, an upper computer 182, a frequency converter 183, a PID controller 184 and a core support a.
Detailed Description
The technical solutions in embodiments 1-3 of the present invention will be clearly and completely described below with reference to fig. 1-2 and specific experimental data, and it is obvious that the described embodiments 1-3 are only a part of embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The following examples 1, 2 and 3 provide a preparation process of environment-friendly discoloration-resistant corrosion-resistant tin plating for chaplet.
Wherein, the first electroplating bath 1 comprises an electroplating bath 11, a constant current/constant potential instrument 12, an anode 13, an electroplating bath heating device 14, a temperature sensor 15, a height adjusting block 16 and a lifting device 17; a first plating solution is contained in the plating tank 11, the pretreated chaplet is used as a cathode and is vertically arranged in the plating tank 11 in parallel with an anode 13, and the anode 13 is a titanium coating anode plate; the anode 13 is connected with the anode of the constant current/potentiostat 12 through an anode line, and the pretreated chaplet is connected with the cathode of the constant current/potentiostat 12 through a cathode line; the plating bath heating device 14 is a snake-shaped titanium alloy heating pipe, and the snake-shaped titanium alloy heating pipe is arranged in the plating bath 11 for heating; a temperature sensor 15 is arranged in the electroplating bath 11; the height adjusting block 16 is arranged in the electroplating bath 11 and is connected with a lifting device 17 positioned outside the electroplating bath 11, and the lifting device 17 is used for adjusting the volume of the height adjusting block 16 immersed in the first plating solution, so that the control of the tin liquid level is realized.
The structure of the second electroplating tank is the same as that of the first electroplating tank 1.
Further, the temperature sensor 15 includes a deep-well thermocouple 151 and a shallow-well thermocouple 152, the deep-well thermocouple 151 is disposed at the bottom of the plating tank 11, and the shallow-well thermocouple 152 is disposed at the upper portion of the plating tank 11. Because the temperature difference exists between the deep groove part and the shallow groove part of the electroplating bath when the core support is in the working state of the electroplating bath 11, the temperature can be quickly adjusted according to the temperature change of tin liquid by arranging the deep groove area thermocouple 151 and the shallow groove area thermocouple 152, and the precision of a temperature control system can be improved.
Further, the first electroplating tank 1 further comprises a control mechanism 18; the control mechanism 18 comprises a PLC181, an upper computer 182, a frequency converter 183 and a PID controller 184, the PLC18 is in communication connection with the upper computer 182, the PLC18 receives and processes signals of the deep groove area thermocouple 151 and the shallow groove area thermocouple 152, the PLC18 receives and processes signals of the constant current/constant potential instrument 12 and controls the constant current/constant potential instrument 12, the PLC18 controls the lifting motor 171 of the lifting device 17 through the frequency converter 183, and the PLC18 controls the serpentine titanium alloy heating pipe through the PID controller 184.
The PLC181 is a central processing unit, Siemens S7-300 and the like can be selected, and the upper computer 182 adopts a touch screen to perform online monitoring on the temperature and the constant current/constant potential rectifier 12 parameters obtained by the PLC and can be controlled through a human-computer interface of the upper computer 182. The PLC181 realizes the precise control of the elevating motor through the frequency converter 183 to control the height of the height adjusting block 16 in the plating tank 11, and when the height adjusting block 16 in the plating tank 11 moves upward or downward, the height of the tin liquid level is controlled by adjusting the volume of the height adjusting block 16 immersed in the tin liquid. The frequency converter 183 can select a Siemens general type frequency converter MicroMaster430, has high reliability and extreme flexibility, can be switched between manual operation and automatic operation, and has the advantage of energy conservation. This converter 183 adopts the electromagnetic compatibility design, and the signal that can quick response gather nevertheless can be fine to quick impulse current's restriction to suffer not due tripping operation scene, influence production in the machine operation.
The plating bath 11 of the invention uses the snakelike titanium alloy heating pipe for heating, and the temperature signal collected by the temperature sensor 15 is sent to the PLC181, the PLC controls the heating pipe in real time through the PID controller 184, thereby heating the bath solution, the PID controller 184 is adopted in the aspect of control, compared with the single closed loop proportion control in the prior art, the dynamic error of temperature control can be eliminated, thereby achieving the purpose of improving the temperature control precision and the stability thereof.
Example 1
(1) Pretreatment: sequentially carrying out pretreatment of chemical oil removal, acid pickling rust removal and activation on the chaplet;
(2) electroplating tin: placing the pretreated chaplet in a first electroplating bath 1, wherein the first electroplating bath contains a first electroplating solution;
(3) cleaning: washing and drying the electroplated chaplet;
(4) electroplating tin: placing the core support into a second electroplating bath, wherein the second electroplating bath is filled with a second plating solution;
(5) cleaning: washing and drying the electroplated chaplet;
(6) anti-discoloration treatment: placing the chaplet into a treatment tank, and soaking for 4min at 15 ℃, wherein the treatment tank is filled with anti-tarnishing treatment liquid;
(7) drying: and drying the chaplet.
The pretreatment specifically comprises the following steps:
(1) Chemical degreasing: cleaning the surface of the core support by adopting deoiling liquid, and washing the surface of the core support by using clear water;
(2) acid pickling for rust removal: pickling the surface of the chaplet by using dilute sulfuric acid with the volume fraction of 5% at room temperature, and washing the surface of the chaplet by using clear water;
(3) activation: and activating the chaplet by adopting a methanesulfonic acid solution.
Wherein the deoiling liquid is prepared from NaOH and Na2CO3、Na3PO4·12H2O、Na2SiO3·9H2O and deionized water, wherein the dosage of NaOH is 65 g.L-1The amount of Na2CO3 used was 25 g.L-1，Na3PO4·12H2The amount of O is 40 g.L-1，Na2SiO3·9H2The amount of O is 6 g.L-1。
Wherein the first plating solution comprises stannous methanesulfonate stock solution, methanesulfonic acid, an additive, 2, 5-dihydroxybenzenesulfonate and deionized water, and the consumption of the stannous methanesulfonate stock solution is 20 g.L-1The amount of methanesulfonic acid used was 45 ml. L-1The dosage of the additive is 5 ml.L-1The antioxidant is 15 ml.L-1. The current density of this electrolytic tin plating was 1.5A dm-2The electroplating time is 2min, and the temperature is 50 ℃.
In addition, the second plating solution comprises tin alkyl sulfonate, alkyl sulfonic acid, a wetting agent, a brightening agent, a stabilizer and deionized water, wherein the dosage of the tin alkyl sulfonate is 45 g.L-1The amount of the alkylsulfonic acid is 125 ml.L-1The dosage of wetting agent is 55 ml.L -1The amount of brightener is 3 ml. L-1The amount of the stabilizer is 4 ml.L-1(ii) a The current density of this electrolytic tin plating was 1.5A dm-2The electroplating time is 2min, and the temperature is 60 ℃.
In addition, the anti-tarnishing treatment fluid comprises phosphoric acid, organic composite acid, corrosion inhibitor, additive and deionized water, wherein the dosage of the phosphoric acid is 15 g.L-1Organic complex acidThe dosage of (B) is 30 g.L-1The dosage of the corrosion inhibitor is 0.3 g.L-1The dosage of the additive is 0.2 g.L-1。
Example 2
(1) Pretreatment: sequentially carrying out pretreatment of chemical oil removal, acid pickling rust removal and activation on the chaplet;
(2) electroplating tin: placing the pretreated chaplet in a first electroplating bath 1, wherein the first electroplating bath contains a first electroplating solution;
(3) cleaning: washing and drying the electroplated chaplet;
(4) electroplating tin: placing the core support into a second electroplating bath, wherein the second electroplating bath is filled with a second plating solution;
(5) cleaning: washing and drying the electroplated chaplet;
(6) anti-discoloration treatment: placing the chaplet in a treatment tank, and soaking for 4min at 50 ℃, wherein the treatment tank is filled with anti-tarnishing treatment liquid;
(7) drying: and drying the chaplet.
The pretreatment specifically comprises the following steps:
(1) Chemical degreasing: cleaning the surface of the core support by adopting deoiling liquid, and washing the surface of the core support by using clear water;
(2) acid pickling for rust removal: pickling the surface of the chaplet by using dilute sulfuric acid with the volume fraction of 5% at room temperature, and washing the surface of the chaplet by using clear water;
(3) activation: and activating the chaplet by adopting a methanesulfonic acid solution.
Wherein the deoiling liquid is prepared from NaOH and Na2CO3、Na3PO4·12H2O、Na2SiO3·9H2O and deionized water, wherein the dosage of NaOH is 75 g.L-1，Na2CO3In an amount of 30 g.L-1，Na3PO4·12H2The amount of O is 35 g.L-1，Na2SiO3·9H2The dosage of O is 8 g.L-1。
Wherein, the first plating solution is a component packageComprises stannous methanesulfonate stock solution, methanesulfonic acid, an additive, 2, 5-dihydroxybenzenesulfonate and deionized water, wherein the dosage of the stannous methanesulfonate stock solution is 22 g.L-1The amount of methanesulfonic acid used was 43 ml. L-1The dosage of the additive is 5 ml.L-1The antioxidant is used in an amount of 20 ml. L-1(ii) a The current density of the electrolytic tinning is 1.4A dm-2The electroplating time is 1.5min, and the temperature is 50 ℃.
In addition, the second plating solution comprises tin alkyl sulfonate, alkyl sulfonic acid, a wetting agent, a brightening agent, a stabilizer and deionized water, wherein the dosage of the tin alkyl sulfonate is 48 g.L-1The amount of the alkylsulfonic acid is 125 ml.L-1The dosage of the wetting agent is 57 ml.L -1The amount of brightener is 5 ml.L-1The amount of the stabilizer is 2 ml.L-1(ii) a The current density of the electrolytic tinning is 1.5A dm-2The electroplating time is 2min, and the temperature is 60 ℃.
In addition, the anti-tarnish treatment liquid comprises phosphoric acid, organic composite acid, corrosion inhibitor, additive and deionized water, wherein the dosage of the phosphoric acid is 12 g.L-1The dosage of the organic composite acid is 35 g.L-1The amount of the corrosion inhibitor is 0.5 g.L-1The dosage of the additive is 0.1 g.L-1。
Example 3
(1) Pretreatment: sequentially carrying out pretreatment of chemical oil removal, acid pickling rust removal and activation on the chaplet;
(2) electroplating tin: placing the pretreated chaplet in a first electroplating bath 1, wherein the first electroplating bath contains a first electroplating solution;
(3) cleaning: washing and drying the electroplated chaplet;
(4) electroplating tin: placing the core support into a second electroplating bath, wherein the second electroplating bath is filled with a second plating solution;
(5) cleaning: washing and drying the electroplated chaplet;
(6) anti-discoloration treatment: placing the chaplet into a treatment tank, and soaking for 4min at 50 ℃, wherein the treatment tank is filled with anti-tarnishing treatment liquid;
(7) drying: and drying the chaplet.
The pretreatment specifically comprises the following steps:
(1) Chemical oil removal: cleaning the surface of the chaplet by adopting deoiling liquid, and then washing the surface of the chaplet by using clear water;
(2) acid pickling for rust removal: pickling the surface of the chaplet by using dilute sulfuric acid with the volume fraction of 5% at room temperature, and washing the surface of the chaplet by using clear water;
(3) and (3) activation: and activating the chaplet by using a methanesulfonic acid solution.
Wherein the deoiling liquid is prepared from NaOH and Na2CO3、Na3PO4·12H2O、Na2SiO3·9H2O and deionized water, wherein the dosage of NaOH is 75 g.L-1，Na2CO3In an amount of 25 g.L-1，Na3PO4·12H2The amount of O is 40 g.L-1，Na2SiO3·9H2The dosage of O is 10 g.L-1。
Wherein the first plating solution comprises stannous methanesulfonate stock solution, methanesulfonic acid, an additive, 2, 5-dihydroxybenzenesulfonate and deionized water, and the consumption of the stannous methanesulfonate stock solution is 22 g.L-1The amount of methanesulfonic acid used was 43 ml. L-1The dosage of the additive is 5 ml.L-1The antioxidant is used in an amount of 20 ml. L-1(ii) a The current density of the electrolytic tinning is 1.5A dm-2The plating time is 1min, and the temperature is 45 ℃.
In addition, the second plating solution comprises tin alkyl sulfonate, alkyl sulfonic acid, a wetting agent, a brightening agent, a stabilizer and deionized water, wherein the dosage of the tin alkyl sulfonate is 50 g.L-1The amount of the alkylsulfonic acid is 120 ml.L-1The dosage of the wetting agent is 65 ml.L-1The amount of brightener is 4 ml. L -1The amount of the stabilizer is 3 ml.L-1(ii) a The current density of the electrolytic tinning is 1.5A dm-2The electroplating time is 2min, and the temperature is 60 ℃.
In addition, the anti-tarnish treatment liquid comprises phosphoric acid and organic complexSynthetic acid, corrosion inhibitor, additive and deionized water, wherein the dosage of phosphoric acid is 14 g.L-1The dosage of the organic composite acid is 32 g.L-1The dosage of the corrosion inhibitor is-0.5 g.L-1The dosage of the additive is 0.2 g.L-1。
Effect verification:
the chaplets obtained in the above examples 1, 2 and 3 and the chaplets without tin plating treatment (comparative example 1) were subjected to performance tests in accordance with the following criteria.
And (3) corrosion resistance testing: (1) 5% saline soaking: the corrosion resistance of the chaplet was tested by a 5% brine soak test. The method comprises the following steps: pouring a prepared 5% saline solution into the beaker, vertically immersing the chaplet sample into the beaker, completely submerging the chaplet sample by the saline solution and keeping a distance of at least 10mm below the level of the saline solution, observing the time of black corrosion spots and yellow corrosion on the surface of the chaplet tin-plated layer, recording the corrosion percentage of the surface of the tin-plated layer, and calculating the corrosion rate; (2) neutral salt spray experiment: the corrosion resistance of the chaplet is detected by a neutral salt spray test. The model of the salt spray box is DCTC1200P, the pH range of 3.5% saline solution of corrosive liquid is 6.7-7.2, the temperature in the box is 33-37 ℃, the core support sample is placed in the salt spray box at an angle of 30-45 degrees with the horizontal, the surface to be tested receives free sedimentation of salt spray, but is not directly sprayed by the core support sample, and the surface appearance of the core support sample is observed and recorded according to the preset time in the experiment.
And (3) aging resistance testing: and (3) performing a steam aging test by referring to a JESD22-A101-D standard, wherein the core support is required to pass the steam aging test when the temperature is 85 ℃ and the humidity RH is 85% for 8h, and the surface of the tin-plated layer of the core support has no color change.
The test results are shown in table 1.
TABLE 1 sample Performance test results
Therefore, the environment-friendly anti-tarnishing and corrosion-resistant tinning preparation process for the chaplet solves the technical problems of larger environmental pollution, poor corrosion resistance effect and poor tarnishing resistance effect of a tinning layer in the chaplet tinning preparation process in the prior art, and greatly improves the corrosion resistance and the tarnishing resistance of the chaplet through secondary tinning electroplating and tarnishing resistance treatment.
The invention has many applications and the above description is only a preferred embodiment of the invention. It should be noted that the above examples are only for illustrating the present invention, and are not intended to limit the scope of the present invention. It will be apparent to those skilled in the art that various modifications can be made without departing from the principles of the invention and these modifications are to be considered within the scope of the invention.
Claims (6)
1. An environment-friendly discoloration-resistant corrosion-resistant tin plating preparation process for a chaplet is characterized by comprising the following steps:
(1) Pretreatment: sequentially carrying out pretreatment of chemical oil removal, acid pickling rust removal and activation on the chaplet; the pretreatment specifically comprises the following steps: 1) chemical oil removal: cleaning the surface of the chaplet by adopting deoiling liquid, and then washing the surface of the chaplet by using clear water; the deoiling liquid is prepared from NaOH and Na2CO3、Na3PO4·12H2O、Na2SiO3·9H2O and deionized water; 2) acid pickling for rust removal: pickling the surface of the chaplet by using dilute sulfuric acid with the volume fraction of 5% at room temperature, and washing the surface of the chaplet by using clear water; 3) and (3) activation: activating the chaplet by adopting a methanesulfonic acid solution;
(2) electroplating tin: placing the pretreated chaplet in a first electroplating bath (1), wherein the first electroplating bath (1) comprises an electroplating bath (11), a constant current/constant potential instrument (12), an anode (13), an electroplating bath heating device (14), a temperature sensor (15), a height adjusting block (16) and a lifting device (17); a first plating solution is contained in the plating tank (11), the pretreated chaplet is used as a cathode and is vertically arranged in the plating tank (11) in parallel with an anode (13), and the anode (13) is a titanium coating anode plate; the anode (13) is connected with the anode of the constant current/constant potential instrument (12) through an anode line, and the pretreated chaplet is connected with the cathode of the constant current/constant potential instrument (12) through a cathode line; the plating bath heating device (14) is a snake-shaped titanium alloy heating pipe, and the snake-shaped titanium alloy heating pipe is arranged in the plating bath (11) for heating; a temperature sensor (15) is arranged in the electroplating bath (11), the temperature sensor (15) comprises a deep-groove-area thermocouple (151) and a shallow-groove-area thermocouple (152), the deep-groove-area thermocouple (151) is arranged at the inner bottom of the electroplating bath (11), and the shallow-groove-area thermocouple (152) is arranged at the inner upper part of the electroplating bath (11); the height adjusting block (16) is arranged in the electroplating bath (11) and is connected with a lifting device (17) positioned outside the electroplating bath (11), and the volume of the height adjusting block (16) immersed in the first plating solution is adjusted through the lifting device (17), so that the height of the tin liquid level is controlled; the first plating solution comprises stannous methanesulfonate stock solution, methanesulfonic acid, an additive, 2, 5-dihydroxybenzenesulfonate and deionized water; the thickness of the tin coating is 0.5-1 μm;
(3) Cleaning: washing and drying the electroplated chaplet;
(4) electroplating tin: placing the core support into a second electroplating bath, wherein the second electroplating bath is filled with a second plating solution; the structure of the second electroplating bath is the same as that of the first electroplating bath (1); the second plating solution comprises tin alkyl sulfonate, alkyl sulfonic acid, a wetting agent, a brightening agent, a stabilizing agent and deionized water; the thickness of the tin coating is 2-4 μm;
(5) cleaning: washing and drying the electroplated chaplet;
(6) anti-discoloration treatment: placing the chaplet in a treatment tank, soaking for 2-5min at 45-55 ℃, wherein the treatment tank is filled with anti-tarnishing treatment liquid; the anti-tarnishing treatment fluid comprises phosphoric acid, organic composite acid, a corrosion inhibitor, an additive and deionized water;
(7) drying: and drying the chaplet.
2. The environmentally friendly anti-tarnishing and corrosion-resistant tin plating preparation process for the chaplet as claimed in claim 1, wherein the amount of NaOH in the deoiling liquid is 60-80 g.L-1，Na2CO3The dosage of the composition is 20-30 g.L-1，Na3PO4·12H2The dosage of O is 30-40 g.L-1， Na2SiO3·9H2The dosage of O is 5-10 g.L-1。
3. The process for preparing environment-friendly anti-tarnishing and corrosion-resistant tin plating for chaplet according to claim 1, wherein the consumption of the stannous methanesulfonate stock solution in the first plating solution is 20-22 g.L -1The dosage of the methanesulfonic acid is 40-45 ml.L-1The dosage of the additive is 4-5 ml.L-1The dosage of the antioxidant is 15-20 ml.L-1(ii) a The electrotinning current density of the step (2) is 1-1.5 A.dm-2The electroplating time is 1-2 min, and the temperature is 40-50 ℃.
4. The process for preparing environment-friendly tarnish-resistant and corrosion-resistant tin plating for chaplet according to claim 1, wherein the amount of tin alkane sulfonate in the plating solution II is 45-50 g.L-1The dosage of the alkyl sulfonic acid is 120-140 ml.L-1The dosage of the wetting agent is 50-70 ml.L-1The amount of brightener is 3-5 ml.L-1The dosage of the stabilizer is 2-4 ml.L-1(ii) a The current density of the electrotinning in the step (4) is 1-1.5 A.dm-2The electroplating time is 1-2 min, and the temperature is 55-60 ℃.
5. The process for preparing environment-friendly discoloration-resistant and corrosion-resistant tin plating for chaplet according to claim 1, wherein the amount of phosphoric acid in said discoloration-resistant treatment liquid is 10 to 15 g.L-1The dosage of the organic composite acid is 30-35 g.L-1Inhibition of corrosionThe dosage of the agent is 0.1-0.5 g.L-1The dosage of the additive is 0.1-0.2 g.L-1。
6. The process for the environmentally friendly discoloration and corrosion resistant tin plating production for chaplet according to claim 1, wherein said plating bath one (1) further comprises a control mechanism (18); the control mechanism (18) comprises a PLC (181), an upper computer (182), a frequency converter (183) and a PID controller (184), the PLC (18) is in communication connection with the upper computer (182), the PLC (18) receives and processes signals of the deep groove area thermocouple (151) and the shallow groove area thermocouple (152), the PLC (18) receives and processes signals of the constant current/potentiostat (12) and controls the constant current/potentiostat (12), the PLC (18) controls a lifting motor (171) of the lifting device (17) through the frequency converter (183), and the PLC (18) controls the snake-shaped titanium alloy heating pipe through the PID controller (184).
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