CN105154938A - Tin and copper carbon nanotube composite coating of automobile terminal, electroplating liquid and electroplating method for tin and copper carbon nanotube composite coating of automobile terminal - Google Patents
Tin and copper carbon nanotube composite coating of automobile terminal, electroplating liquid and electroplating method for tin and copper carbon nanotube composite coating of automobile terminal Download PDFInfo
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- CN105154938A CN105154938A CN201510505088.7A CN201510505088A CN105154938A CN 105154938 A CN105154938 A CN 105154938A CN 201510505088 A CN201510505088 A CN 201510505088A CN 105154938 A CN105154938 A CN 105154938A
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Abstract
The invention discloses a tin and copper carbon nanotube composite coating of an automobile terminal, electroplating liquid and an electroplating method for the tin and copper carbon nanotube composite coating of the automobile terminal. The thickness of the coating is 0.5 micrometers, and the coating is prepared from, by mass, 1-3% of copper, 0.2-0.8% of carbon nanotube and the balance tin. The electroplating liquid is prepared from 30 g/L of tin sulfate, 3 g/L of copper sulfate, 50 g/L of citric acid, 35 g/L of tartaric acid, 100 mL/L of 98% sulfuric acid, 0.4 mg/L of 2-mercapto benzimidazole, 0.1g/L of sodium dodecyl sulfate and 1g/L of carbon nanotube. The treated automobile terminal is electroplated for 8-12 minutes in the electroplating liquid at 25 DEG C with the cathode-current density of 3 A/dm<2> and the rolling speed of 8 turns per minute. The problems that the plugging force of the automobile terminal obtained after tin plating is increased too much and assembling is difficult are solved, and the electroplating processes and the thickness of the coating are reduced; and while the cost is reduced, the plugging force is reduced, the protection performance of the terminal is improved, and the capability of resisting zinc diffusion which causes color changing of the coating is improved.
Description
Technical field
The invention belongs to automobile terminal preparing technical field, be specifically related to a kind of preparation method of automobile terminal tin copper carbon nanotubes composite coatings.
Background technology
Automobile terminal mainly adopts brass or bronze material, under the environment of moist or high temperature, easily oxidation stain contact resistance raises and affects terminal electroconductibility, for solving the problem of oxidation of terminal, at present main what adopt is the tin protective layer electroplating the comparatively strong and good conductivity of antioxidant property power on automobile terminal, and brass base needs the copper of preplating 0.5 micron or nickel coating to prevent the diffusion of zinc in brass base from causing tin coating variable color.But due to tin coating hardness lower, frictional coefficient result in greatly while raising terminal protective capacities, the contact engaging and separating force of plated terminals improves, result in the difficulty of automobile terminal assembling, easily there is variable color in the situation of zinc diffusion in tin coating, brass base need increase the copper of preplating 0.5 micron or nickel coating operation causes tin coating discoloration problem to prevent the diffusion of zinc in brass base.
Summary of the invention
Technical problem to be solved by this invention is for problems of the prior art, a kind of automobile terminal tin copper carbon nanotubes composite coatings, electroplate liquid and electro-plating method thereof are provided, solving the zinc-plated rear contact engaging and separating force of automobile terminal increases excessive, the problem of assembling difficulty, decrease electroplating work procedure and thickness of coating, while reducing costs, reduce contact engaging and separating force, improve the ability that the barrier propterty of terminal and anti-zinc diffuse to coating color.
For solving the problems of the technologies described above, the present invention by the following technical solutions:
A kind of automobile terminal tin copper carbon nanotubes composite coatings, this thickness of coating is 0.5 micron, and the mass percent of each component of this coating is as follows: copper 1 ~ 3%, carbon nanotube 0.2 ~ 0.8%, and all the other are tin.
Described automobile terminal tin copper carbon nanotubes composite coatings, the mass percent of each component of this coating is as follows: copper 2%, carbon nanotube 0.5%, and all the other are tin.
The electroplate liquid that a kind of automobile terminal tin copper carbon nanotubes composite coatings adopts, fill a prescription as follows: stannous sulfate 25 ~ 35g/L, copper sulfate 1 ~ 5g/L, citric acid 45 ~ 55g/L, tartrate 30 ~ 40g/L, 98% sulfuric acid 95 ~ 105mL/L, 2-mercaptobenzimidazole 0.1 ~ 0.6mg/L, sodium laurylsulfonate 0.05 ~ 0.2g/L, carbon nanotube 0.5 ~ 1.5g/L.
The electroplate liquid that described automobile terminal tin copper carbon nanotubes composite coatings adopts, fills a prescription as follows: stannous sulfate 30g/L, copper sulfate 3g/L, citric acid 50g/L, tartrate 35g/L, 98% sulfuric acid 100mL/L, 2-mercaptobenzimidazole 0.4mg/L, sodium laurylsulfonate 0.1g/L, carbon nanotube 1g/L.
An electro-plating method for automobile terminal tin copper carbon nanotubes composite coatings, step is as follows:
(1) in the coating bath cleaned, add deionized water, slowly add 98% sulfuric acid, after solution is chilled to 25 ~ 35 DEG C, adds stannous sulfate, copper sulfate, citric acid, tartrate and 2-mercaptobenzimidazole, and be constantly stirred to dissolve wiring solution-forming A;
(2) sodium lauryl sulphate and carbon nanotube are added in deionized water, by ultrasonic wave dispersion 8 ~ 15 minutes wiring solution-forming B;
(3) solution B is added in solution A, hang tin anode and corrugated type electrolytic iron negative plate, and through 1.5 ~ 2.5 hours low current electrolysis treatment, obtain electroplate liquid, wherein the concentration of each component is: stannous sulfate 25 ~ 35g/L, copper sulfate 1 ~ 5g/L, citric acid 45 ~ 55g/L, tartrate 30 ~ 40g/L, 98% sulfuric acid 95 ~ 105mL/L, 2-mercaptobenzimidazole 0.1 ~ 0.6mg/L, sodium laurylsulfonate 0.05 ~ 0.2g/L, carbon nanotube 0.5 ~ 1.5g/L;
(4) automobile terminal is added cylinder through 3 ~ 8 minutes ultrasonic oil removal, 10% after sulfuric acid activated 3 ~ 8 seconds, in the electroplate liquid of 25 DEG C, cathode current density 3A/dm
2and plating 8 ~ 12 minutes (time increases thickness of coating and extends, and obtains the nano-pipe compound plated layer of even tin copper in terminal surfaces) under rolling the condition of speed 8 revs/min.
In described step (1) deionized water volume+step (2) in the cumulative volume of deionized water of volume=required of deionized water.
In described step (1) deionized water volume+step (2) in the cumulative volume of the deionized water required for volume < of deionized water time, in step (3) solution B is added in solution A, and then adds deionized water to volume required.
Beneficial effect of the present invention: the codeposition 1, adopting the complexing of citric acid and tartrate and copper to achieve tin and copper adds the hardness of tin coating, reduces the contact engaging and separating force of coating.2, carbon nanotube ultrasonic wave will disperse in advance in zinc-plated dispersion agent sodium laurylsulfonate, and rolled with the rotating speed of 8 revs/min by cylinder, prevent its sedimentation, achieve the codeposition with tin copper, improve lubricity and the electroconductibility of coating, reduce contact engaging and separating force, improve the barrier propterty of coating.3, the present invention adopts 0.5 micron of tin copper carbon nano-composite plate to instead of traditional 0.5 micron of copper coating+2 microns of tin coatings, when reduce operation, reduce costs zinc diffusion can not cause coating color.4, it is theoretical that the present invention adopts TRIZ(inventive problem to solve in triturating) in cutting rule cropped auxiliary copper facing operation, by a large amount of tests, copper is incorporated in tin coating the hardness improving coating, simultaneously by analyzing the trend of evolution of this technological system zinc-plated, judge that it is in the ripening stage according to multiple data, technological system microevolution rule can be adopted in the ripening stage---the evolution of technological system is along the future development reducing its component size, namely element is from initial size to atom, the size of ultimate particle is evolved, better can realize identical function solves coating Problems existing simultaneously, visualize and adopt the composite deposite of tin copper carbon nanotube to replace tin coating, and finally obtain carbon nanotubes composite coatings by multiple test, it has better anti-tarnishing ability, electroconductibility and lubricity.
Accompanying drawing explanation
Fig. 1 is the XRF energy spectrogram of the embodiment of the present invention 4 coating.
Embodiment
Embodiment 1
The electroplate liquid that automobile terminal tin copper carbon nanotubes composite coatings adopts, fills a prescription as follows: stannous sulfate 25g/L, copper sulfate 5g/L, citric acid 45g/L, tartrate 40g/L, 98% sulfuric acid 95mL/L, 2-mercaptobenzimidazole 0.6mg/L, sodium laurylsulfonate 0.05g/L, carbon nanotube 1.5g/L.
An electro-plating method for automobile terminal tin copper carbon nanotubes composite coatings, step is as follows:
(1) in the coating bath cleaned, add deionized water, slowly add 98% sulfuric acid, after solution is chilled to 25 DEG C, adds stannous sulfate, copper sulfate, citric acid, tartrate and 2-mercaptobenzimidazole, and be constantly stirred to dissolve wiring solution-forming A;
(2) sodium lauryl sulphate and carbon nanotube are added in deionized water, disperse 8 minutes wiring solution-forming B by ultrasonic wave;
(3) solution B is added in solution A, hang tin anode and corrugated type electrolytic iron negative plate, and through 1.5 hours low current electrolysis treatment, obtain electroplate liquid;
(4) automobile terminal is added cylinder through 3 minutes ultrasonic oil removal, 10% after sulfuric acid activated 8 seconds, in the electroplate liquid of 25 DEG C, cathode current density 3A/dm
2and electroplate 8 minutes under rolling the condition of speed 8 revs/min.
Embodiment 2
The electroplate liquid that automobile terminal tin copper carbon nanotubes composite coatings adopts, fills a prescription as follows: stannous sulfate 35g/L, copper sulfate 1g/L, citric acid 55g/L, tartrate 30g/L, 98% sulfuric acid 105mL/L, 2-mercaptobenzimidazole 0.1mg/L, sodium laurylsulfonate 0.2g/L, carbon nanotube 0.5g/L.
An electro-plating method for automobile terminal tin copper carbon nanotubes composite coatings, step is as follows:
(1) in the coating bath cleaned, add deionized water, slowly add 98% sulfuric acid, after solution is chilled to 35 DEG C, adds stannous sulfate, copper sulfate, citric acid, tartrate and 2-mercaptobenzimidazole, and be constantly stirred to dissolve wiring solution-forming A;
(2) sodium lauryl sulphate and carbon nanotube are added in deionized water, disperse 15 minutes wiring solution-forming B by ultrasonic wave;
(3) solution B is added in solution A, now, if the total amount of step (1) and the middle deionized water of step (2) fails to reach required volume, then need to add deionized water, make it to reach required volume, then tin anode and corrugated type electrolytic iron negative plate is hung, and through 2.5 hours low current electrolysis treatment, obtain electroplate liquid;
(4) automobile terminal is added cylinder through 3 ~ 8 minutes ultrasonic oil removal, 10% after sulfuric acid activated 3 ~ 8 seconds, in the electroplate liquid of 25 DEG C, cathode current density 3A/dm
2and plating 8 ~ 12 minutes (time increases thickness of coating and extends, and obtains the nano-pipe compound plated layer of even tin copper in terminal surfaces) under rolling the condition of speed 8 revs/min.
Embodiment 3
The electroplate liquid that automobile terminal tin copper carbon nanotubes composite coatings adopts, fills a prescription as follows: stannous sulfate 30g/L, copper sulfate 3g/L, citric acid 50g/L, tartrate 35g/L, 98% sulfuric acid 100mL/L, 2-mercaptobenzimidazole 0.4mg/L, sodium laurylsulfonate 0.1g/L, carbon nanotube 1g/L.
An electro-plating method for automobile terminal tin copper carbon nanotubes composite coatings, step is as follows:
(1) in the coating bath cleaned, deionized water 60L is added, slowly add 98% sulfuric acid, after solution is chilled to 30 DEG C, adds 30g stannous sulfate, 3g/ copper sulfate, 50g citric acid, 35g tartrate and 0.4mg2-mercaptobenzimidazole, and is constantly stirred to dissolve wiring solution-forming A;
(2) 0.1g sodium lauryl sulphate and 1g carbon nanotube are added in 5L deionized water, disperse 10 minutes wiring solution-forming B by ultrasonic wave;
(3) solution B is added in solution A, and then add 35L deionized water, hang tin anode and corrugated type electrolytic iron negative plate, and through 2 hours low current electrolysis treatment, obtain electroplate liquid;
(4) automobile terminal is added cylinder through 5 minutes ultrasonic oil removal, 10% after sulfuric acid activated 5 seconds, in the electroplate liquid of 25 DEG C, cathode current density 3A/dm
2and plating 10 minutes under rolling the speed condition of 8 revs/min, obtain tin copper carbon nanotubes composite coatings thickness be 5 microns, wherein each component concentration is copper 2%, carbon nanotube 0.5%, and all the other are tin.
Embodiment 4
By plating solution formula and electro-plating method in embodiment 3, getting the manufacture of H65 brass material has locking latches DJ621-6.3A plug and each 3 kilograms of DJ621-6.3B socket to put into cylinder respectively and carry out electro-coppering sijna mitron composite deposite 0.5 micron.The composition adopting XRF energy spectrometer to determine coating is copper 2.0%, tin 97.5, carbon 0.5%.Can spectrogram as indicated with 1.
Measure according to the mensuration of automobile industry standard QC/T417-2001 second section 4.3 insertion force and withdrawal force, 4.16 salt-fog tests, 4.8 contact resistances survey its insertion force, withdrawal force, etch resistant properties, contact resistance, in the baking oven of 150 degree, placement measures its anti-matrix zinc thermodiffusion experimental examination coating discoloration-resisting for 10 hours.Adopt DJ621-6.3A plug and the DJ621-6.3B socket of zinc-plated 2 microns or 2 microns, Direct Electroplating tin after copper facing 0.5 micron simultaneously, adopt same procedure to measure its insertion force, contact engaging and separating force, etch resistant properties, contact resistance and anti-zinc diffusibility, the terminal performance of its result and Direct Electroplating copper sijna mitron composite deposite 0.5 micron carries out contrast as following table.
| Brass DJ621-6.3 plug, socket coating conditions | First time insertion force N | First time withdrawal force N | Contact resistance milliohm after first grafting | 48 hours salt-fog tests | 150 degree of thermodiffusion in 10 hours tests |
| Without coating | 32.1 | 31.5 | 4.3 | There is obvious brown oxidation spot in 50% brass base surface | At high temperature there is white oxide film in brass base surface 90% |
| 0.5 micron of nano-pipe compound plated layer of tin copper | 32.8 | 31.9 | 3.1 | Coating does not find corrosion | Coating silvery white is unchanged |
| 2 microns of tin coatings | 42.8 | 43.9 | 3.7 | Corrosion of coating area 10% | Tin coating grey |
| 0.5 micron of copper coating+2 microns of tin coatings | 44．2 | 44.7 | 3.8 | Corrosion of coating area is less than 3% | Coating is without considerable change |
On automobile terminal, electroplating 0.5 micron of nano-pipe compound plated layer of tin copper as can be known from the above table, not only the insertion of terminal and withdrawal force reduce more than 10N than the insertion force withdrawal force of tin and copper+tin coating, with compared with coating terminal without considerable change, simultaneously contact resistance also has certain reduction; Salt-fog test result shows that its corrosion stability is more than 0.5 micron of copper coating+2 microns of tin coatings; Anti-zinc expanding metachrosis is good, consistent with 0.5 micron of copper coating+2 microns of tin coatings, showing that 0.5 micron of nano-pipe compound plated layer of tin copper can have the contact resistance of reduction, good etch resistant properties and anti-zinc diffusion metachrosis when reducing contact engaging and separating force, under the operation saving plating 0.5 micron of copper, improve the correlated performance of plated terminals.
Claims (7)
1. an automobile terminal tin copper carbon nanotubes composite coatings, is characterized in that: this thickness of coating is 0.5 micron, and the mass percent of each component of this coating is as follows: copper 1 ~ 3%, carbon nanotube 0.2 ~ 0.8%, and all the other are tin.
2. automobile terminal tin copper carbon nanotubes composite coatings according to claim 1, is characterized in that: the mass percent of each component of this coating is as follows: copper 2%, carbon nanotube 0.5%, all the other are tin.
3. the electroplate liquid of automobile terminal tin copper carbon nanotubes composite coatings employing according to claim 1, it is characterized in that formula is as follows: stannous sulfate 25 ~ 35g/L, copper sulfate 1 ~ 5g/L, citric acid 45 ~ 55g/L, tartrate 30 ~ 40g/L, 98% sulfuric acid 95 ~ 105mL/L, 2-mercaptobenzimidazole 0.1 ~ 0.6mg/L, sodium laurylsulfonate 0.05 ~ 0.2g/L, carbon nanotube 0.5 ~ 1.5g/L.
4. the electroplate liquid of automobile terminal tin copper carbon nanotubes composite coatings employing according to claim 3, it is characterized in that formula is as follows: stannous sulfate 30g/L, copper sulfate 3g/L, citric acid 50g/L, tartrate 35g/L, 98% sulfuric acid 100mL/L, 2-mercaptobenzimidazole 0.4mg/L, sodium laurylsulfonate 0.1g/L, carbon nanotube 1g/L.
5. adopt electroplate liquid according to claim 2 to form the electro-plating method of automobile terminal tin copper carbon nanotubes composite coatings according to claim 1, it is characterized in that step is as follows:
(1) in the coating bath cleaned, add deionized water, slowly add 98% sulfuric acid, after solution is chilled to 25 ~ 35 DEG C, adds stannous sulfate, copper sulfate, citric acid, tartrate and 2-mercaptobenzimidazole, and be constantly stirred to dissolve wiring solution-forming A;
(2) sodium lauryl sulphate and carbon nanotube are added in deionized water, by ultrasonic wave dispersion 8 ~ 15 minutes wiring solution-forming B;
(3) solution B is added in solution A, hang tin anode and corrugated type electrolytic iron negative plate, and through 1.5 ~ 2.5 hours low current electrolysis treatment, obtain electroplate liquid, wherein the concentration of each component is: stannous sulfate 25 ~ 35g/L, copper sulfate 1 ~ 5g/L, citric acid 45 ~ 55g/L, tartrate 30 ~ 40g/L, 98% sulfuric acid 95 ~ 105mL/L, 2-mercaptobenzimidazole 0.1 ~ 0.6mg/L, sodium laurylsulfonate 0.05 ~ 0.2g/L, carbon nanotube 0.5 ~ 1.5g/L;
(4) automobile terminal is added cylinder through 3 ~ 8 minutes ultrasonic oil removal, 10% after sulfuric acid activated 3 ~ 8 seconds, in the electroplate liquid of 25 DEG C, cathode current density 3A/dm
2and electroplate 8 ~ 12 minutes under rolling the condition of speed 8 revs/min.
6. the electro-plating method of automobile terminal tin copper carbon nanotubes composite coatings according to claim 5, is characterized in that: in described step (1) deionized water volume+step (2) in the cumulative volume of deionized water of volume=required of deionized water.
7. the electro-plating method of automobile terminal tin copper carbon nanotubes composite coatings according to claim 5, it is characterized in that: in described step (1) deionized water volume+step (2) in the cumulative volume of the deionized water required for volume < of deionized water time, in step (3) solution B is added in solution A, and then add deionized water to volume required.
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| CN101866721A (en) * | 2009-04-15 | 2010-10-20 | 韩国科学技术研究院 | Method for fabrication of conductive film using conductive frame and conductive film |
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