CN105154938B - Automobile terminal stannum copper carbon nanotubes composite coatings, electroplate liquid and electro-plating method thereof - Google Patents

Automobile terminal stannum copper carbon nanotubes composite coatings, electroplate liquid and electro-plating method thereof Download PDF

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CN105154938B
CN105154938B CN201510505088.7A CN201510505088A CN105154938B CN 105154938 B CN105154938 B CN 105154938B CN 201510505088 A CN201510505088 A CN 201510505088A CN 105154938 B CN105154938 B CN 105154938B
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copper
stannum
cnt
automobile terminal
deionized water
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CN105154938A (en
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赵平堂
张景堂
覃洪
张献军
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Henan THB Electric Co Ltd
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Henan THB Electric Co Ltd
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Abstract

The invention discloses a kind of automobile terminal stannum copper carbon nanotubes composite coatings, electroplate liquid and electro-plating method thereof, thickness of coating is 0.5 micron, and the mass percent of each component is as follows: copper 1 ~ 3%, CNT 0.2 ~ 0.8%, and remaining is stannum;Electroplate liquid is as follows: stannous sulfate 30g/L, copper sulfate 3g/L, citric acid 50g/L, tartaric acid 35g/L, 98% sulphuric acid 100mL/L, 2 mercaptobenzimidazole 0.4mg/L, dodecyl sodium sulfate 0.1g/L, CNT 1g/L.The automobile terminal after process in the electroplate liquid of 25 DEG C, cathode-current density 3A/dm2, rolling speed 8 revs/min electroplate 8 ~ 12 minutes, solve the tin plating rear contact engaging and separating force of automobile terminal and increase excessive, the problem of assembling difficulty, decreases electroplating work procedure and thickness of coating, reduces contact engaging and separating force, the barrier propterty that improve terminal and anti-zinc and diffuse to the ability of coating color while reducing cost.

Description

Automobile terminal stannum copper carbon nanotubes composite coatings, electroplate liquid and electro-plating method thereof
Technical field
The invention belongs to automobile terminal preparing technical field, be specifically related to a kind of automobile terminal stannum copper CNT Composite Coatings The preparation method of layer.
Background technology
Automobile terminal mainly uses pyrite or bronze material, and in the environment of humidity or high temperature, easily oxidation stain contact is electric Resistance raises and affects terminal electric conductivity, for solving the problem of oxidation of terminal, currently mainly uses and electroplates on automobile terminal Non-oxidizability ability is relatively strong and the stannum overcoat of good conductivity, and brass base needs the copper of preplating 0.5 micron or nickel coating to prevent Huang In Copper substrate, the diffusion of zinc causes tin coating variable color.Relatively low yet with tin coating hardness, coefficient of friction result in greatly and improving While terminal protective capacities, the contact engaging and separating force of plated terminals improves, and result in the difficulty of automobile terminal assembling, and tin coating easily exists There is variable color in the situation of zinc diffusion, and brass base need to increase the copper of preplating 0.5 micron or nickel coating operation to prevent brass base The diffusion of middle zinc causes tin coating discoloration problem.
Summary of the invention
The technical problem to be solved is for problems of the prior art, it is provided that a kind of automobile end Sub-stannum copper carbon nanotubes composite coatings, electroplate liquid and electro-plating method thereof, solving the tin plating rear contact engaging and separating force of automobile terminal increases excessive, The problem of assembling difficulty, decreases electroplating work procedure and thickness of coating, reduces contact engaging and separating force, improves end while reducing cost The barrier propterty of son and anti-zinc diffuse to the ability of coating color.
For solve above-mentioned technical problem, the present invention by the following technical solutions:
A kind of automobile terminal stannum copper carbon nanotubes composite coatings, this thickness of coating is 0.5 micron, the matter of each component of this coating Amount percentage ratio is as follows: copper 1 ~ 3%, CNT 0.2 ~ 0.8%, remaining is stannum.
Described automobile terminal stannum copper carbon nanotubes composite coatings, the mass percent of each component of this coating is as follows: copper 2%, CNT 0.5%, remaining is stannum.
The electroplate liquid that a kind of automobile terminal stannum copper carbon nanotubes composite coatings uses, formula is as follows: stannous sulfate 25 ~ 35g/L, copper sulfate 1 ~ 5g/L, citric acid 45 ~ 55g/L, tartaric acid 30 ~ 40g/L, 98% sulphuric acid 95 ~ 105mL/L, 2-sulfydryl benzo Imidazoles 0.1 ~ 0.6mg/L, dodecyl sodium sulfate 0.05 ~ 0.2g/L, CNT 0.5 ~ 1.5g/L.
The electroplate liquid that described automobile terminal stannum copper carbon nanotubes composite coatings uses, formula is as follows: stannous sulfate 30g/ L, copper sulfate 3 g/L, citric acid 50g/L, tartaric acid 35g/L, 98% sulphuric acid 100mL/L, 2-mercaptobenzimidazole 0.4mg/ L, dodecyl sodium sulfate 0.1 g/L, CNT 1g/L.
A kind of electro-plating method of automobile terminal stannum copper carbon nanotubes composite coatings, step is as follows:
(1) in clean coating bath, add deionized water, be slowly added into 98% sulphuric acid, add after solution is cooled to 25 ~ 35 DEG C Stannous sulfate, copper sulfate, citric acid, tartaric acid and 2-mercaptobenzimidazole, and constantly it is stirred to dissolve wiring solution-forming A;
(2) dodecyl sodium sulfate and CNT are added in deionized water, within 8 ~ 15 minutes, joined by ultrasound wave dispersion Become solution B;
(3) solution B is added in solution A, hang tin anode and corrugated type electrolytic iron minus plate, and little through 1.5 ~ 2.5 Time low current electrolysis process, obtain electroplate liquid, the concentration of the most each component is: stannous sulfate 25 ~ 35g/L, copper sulfate 1 ~ 5g/ L, citric acid 45 ~ 55g/L, tartaric acid 30 ~ 40g/L, 98% sulphuric acid 95 ~ 105mL/L, 2-mercaptobenzimidazole 0.1 ~ 0.6mg/L, Dodecyl sodium sulfate 0.05 ~ 0.2g/L, CNT 0.5 ~ 1.5g/L;
(4) automobile terminal through 3 ~ 8 minutes ultrasonic oil removal, 10% add cylinder, at 25 DEG C after sulfuric acid activated 3 ~ 8 seconds Electroplate liquid in, cathode-current density 3A/dm2And (time increases coating thickness to electroplate 8 ~ 12 minutes under conditions of rolling speed 8 revs/min Degree extends, and obtains the uniform nano-pipe compound plated layer of stannum copper in terminal surfaces).
The deionized water of the volume of deionized water in the volume+step (2) of deionized water in described step (1)=required Cumulative volume.
Volume < the required deionized water of deionized water in the volume+step (2) of deionized water in described step (1) Cumulative volume time, in step (3) solution B is added in solution A, adds deionized water the most again to the most volume required.
Beneficial effects of the present invention: 1, use the complexation of citric acid and tartaric acid and copper to achieve the codeposition increasing of stannum and copper Add the hardness of tin coating, reduce the contact engaging and separating force of coating.2, CNT in advance will be at tin plating dispersant dodecyl sodium sulfonate Ultrasound wave dispersion in sodium, and being rolled with the rotating speed of 8 revs/min by cylinder, prevents it from settling, it is achieved that with the codeposition of stannum copper, Improve lubricating ability and the electric conductivity of coating, reduce contact engaging and separating force, improve the barrier propterty of coating.3, the present invention uses 0.5 micron of stannum copper carbon nano-composite plate instead of traditional 0.5 micron+2 microns of tin coatings of copper coating, is reducing operation, fall In the case of low cost, zinc diffusion is not result in coating color.4, the present invention uses TRIZ(inventive problem solution in development process Certainly theory) in cutting rule cropped the copper facing operation of auxiliary, by substantial amounts of test copper is incorporated in tin coating and carries According to multiple data, the hardness of high coating, simultaneously by analyzing the trend of evolution of this technological system tin plating, judges that it is in In the period of maturation, the evolution that can use technological system microevolution rule technological system in the period of maturation is along reducing its element The direction of size is developed, i.e. element is evolved to atom, the size of fundamental particle from initial size, simultaneously can be preferably real Existing identical function solves the problem that coating exists, and visualizes and uses the composite deposite of stannum copper CNT to replace tin coating, And it being finally obtained carbon nanotubes composite coatings by multiple test, it has more preferable anti-tarnishing ability, electric conductivity and lubrication Ability.
Accompanying drawing explanation
Fig. 1 is the XRF energy spectrogram of the embodiment of the present invention 4 coating.
Detailed description of the invention
Embodiment 1
The electroplate liquid that a kind of automobile terminal stannum copper carbon nanotubes composite coatings uses, formula is as follows: stannous sulfate 25g/L, Copper sulfate 5g/L, citric acid 45g/L, tartaric acid 40g/L, 98% sulphuric acid 95mL/L, 2-mercaptobenzimidazole 0.6mg/L, dodecane Base sodium sulfonate 0.05g/L, CNT 1.5g/L.
A kind of electro-plating method of automobile terminal stannum copper carbon nanotubes composite coatings, step is as follows:
(1) in clean coating bath, add deionized water, be slowly added into 98% sulphuric acid, after solution is cooled to 25 DEG C, adds sulfur Acid stannous, copper sulfate, citric acid, tartaric acid and 2-mercaptobenzimidazole, and constantly it is stirred to dissolve wiring solution-forming A;
(2) dodecyl sodium sulfate and CNT are added in deionized water, within 8 minutes, be made into molten by ultrasound wave dispersion Liquid B;
(3) solution B is added in solution A, hang tin anode and corrugated type electrolytic iron minus plate, and low through 1.5 hours Current electroanalysis processes, and obtains electroplate liquid;
(4) automobile terminal through 3 minutes ultrasonic oil removal, 10% add cylinder, at the electricity of 25 DEG C after sulfuric acid activated 8 seconds In plating solution, cathode-current density 3A/dm2And electroplate 8 minutes under conditions of rolling speed 8 revs/min.
Embodiment 2
The electroplate liquid that a kind of automobile terminal stannum copper carbon nanotubes composite coatings uses, formula is as follows: stannous sulfate 35g/L, Copper sulfate 1g/L, citric acid 55g/L, tartaric acid 30g/L, 98% sulphuric acid 105mL/L, 2-mercaptobenzimidazole 0.1mg/L, 12 Sodium alkyl sulfonate 0.2g/L, CNT 0.5g/L.
A kind of electro-plating method of automobile terminal stannum copper carbon nanotubes composite coatings, step is as follows:
(1) in clean coating bath, add deionized water, be slowly added into 98% sulphuric acid, after solution is cooled to 35 DEG C, adds sulfur Acid stannous, copper sulfate, citric acid, tartaric acid and 2-mercaptobenzimidazole, and constantly it is stirred to dissolve wiring solution-forming A;
(2) dodecyl sodium sulfate and CNT are added in deionized water, within 15 minutes, be made into by ultrasound wave dispersion Solution B;
(3) solution B is added in solution A, now, if the total amount of deionized water fails to reach in step (1) and step (2) Required volume, then need to add deionized water, makes up to required volume, then hangs tin anode and corrugated type ferroelectricity Solve minus plate, and process through low current electrolysis in 2.5 hours, obtain electroplate liquid;
(4) automobile terminal through 3 ~ 8 minutes ultrasonic oil removal, 10% add cylinder, at 25 DEG C after sulfuric acid activated 3 ~ 8 seconds Electroplate liquid in, cathode-current density 3A/dm2And (time increases coating thickness to electroplate 8 ~ 12 minutes under conditions of rolling speed 8 revs/min Degree extends, and obtains the uniform nano-pipe compound plated layer of stannum copper in terminal surfaces).
Embodiment 3
The electroplate liquid that a kind of automobile terminal stannum copper carbon nanotubes composite coatings uses, formula is as follows: stannous sulfate 30g/L, Copper sulfate 3g/L, citric acid 50g/L, tartaric acid 35g/L, 98% sulphuric acid 100mL/L, 2-mercaptobenzimidazole 0.4mg/L, ten Dialkyl sulfonates 0.1 g/L, CNT 1g/L.
A kind of electro-plating method of automobile terminal stannum copper carbon nanotubes composite coatings, step is as follows:
(1) in clean coating bath, add deionized water 60L, be slowly added into 98% sulphuric acid, add after solution is cooled to 30 DEG C 30g stannous sulfate, 3g/ copper sulfate, 50g citric acid, 35g tartaric acid and 0.4mg 2-mercaptobenzimidazole, and be stirred continuously and make Dissolve wiring solution-forming A;
(2) 0.1 g dodecyl sodium sulfate and 1g CNT are added in 5L deionized water, disperse 10 by ultrasound wave Minute wiring solution-forming B;
(3) solution B is added in solution A, then add 35L deionized water, hang tin anode and corrugated type electrolytic iron Minus plate, and process through low current electrolysis in 2 hours, obtain electroplate liquid;
(4) automobile terminal through 5 minutes ultrasonic oil removal, 10% add cylinder, at the electricity of 25 DEG C after sulfuric acid activated 5 seconds In plating solution, cathode-current density 3A/dm2And electroplate 10 minutes under conditions of rolling speed 8 revs/min, obtain stannum copper CNT and be combined Coating thickness be 5 microns, the most each constituent content is copper 2%, CNT 0.5%, and remaining is stannum.
Embodiment 4
By plating solution formula and electro-plating method in embodiment 3, taking H65 brass material manufacture has locking device DJ621-6.3A Plug and each 3 kilograms of DJ621-6.3B socket are respectively put into cylinder and carry out electro-coppering sijna mitron composite deposite 0.5 micron.Use It is copper 2.0% that XRF energy disperse spectroscopy determines the composition of coating, stannum 97.5, carbon 0.5%.Energy spectrogram is as the most as indicated with 1.
According to automobile industry standard QC/T417-2001 Part II 4.3 insertion force and the mensuration of withdrawal force, 4.16 salt fogs Test determination, 4.8 contact resistances survey its insertion force, withdrawal force, etch resistant properties, contact resistance, place 10 in the baking oven of 150 degree Hour measure its anti-matrix zinc thermal diffusion experimental examination coating discoloration-resisting.Use after copper facing 0.5 micron tin plating 2 microns simultaneously Or the DJ621-6.3A plug of 2 microns of Direct Electroplating stannum and DJ621-6.3B socket, use same procedure to measure its insertion force, insert Pull out force, etch resistant properties, contact resistance and anti-zinc diffusivity, its result layer nano-pipe compound plated with Direct Electroplating copper and tin 0.5 is micro- The terminal performance of rice carries out contrast such as following table.
Pyrite DJ621-6.3 plug, socket coating conditions Insertion force N for the first time Withdrawal force N for the first time Contact resistance milliohm after first grafting 48 hours salt spray tests 150 degree of thermal diffusion in 10 hours tests
Without coating 32.1 31.5 4.3 There is obvious brown oxidation speckle 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 stannum copper 32.8 31.9 3.1 Coating does not finds 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
+ 2 microns of tin coatings of 0.5 micron of copper coating 44.2 44.7 3.8 Corrosion of coating area is less than 3% Coating is without significant change
On automobile terminal, electroplate the insertion of 0.5 micron of stannum copper nano-pipe compound plated layer not only terminal as can be known from the above table and pull out Exert oneself ratio stannum and copper+tin coating insertion force withdrawal force reduce more than 10N, with compared with coating terminal without significant change, simultaneously Contact resistance also has certain reduction;Salt spray test result shows that its corrosion stability is more than+2 microns of tin coatings of 0.5 micron of copper coating;Anti- Zinc expanding metachrosis is good, consistent with+2 microns of tin coatings of 0.5 micron of copper coating, shows that 0.5 micron of stannum copper is nano-pipe compound plated Layer can have the contact resistance of reduction, good etch resistant properties and anti-zinc diffusion variable color energy in the case of reducing contact engaging and separating force Power, improves the correlated performance of plated terminals under the operation saving 0.5 micron of copper of plating.

Claims (7)

1. an automobile terminal stannum copper carbon nanotubes composite coatings, it is characterised in that: this thickness of coating is 0.5 micron, this coating The mass percent of each component is as follows: copper 1 ~ 3%, CNT 0.2 ~ 0.8%, and remaining is stannum.
Automobile terminal stannum copper carbon nanotubes composite coatings the most according to claim 1, it is characterised in that: each component of this coating Mass percent as follows: copper 2%, CNT 0.5%, remaining be stannum.
3. the electroplate liquid that the automobile terminal stannum copper carbon nanotubes composite coatings described in claim 1 uses, it is characterised in that formula As follows: stannous sulfate 25 ~ 35g/L, copper sulfate 1 ~ 5g/L, citric acid 45 ~ 55g/L, tartaric acid 30 ~ 40g/L, 98% sulphuric acid 95 ~ 105mL/L, 2-mercaptobenzimidazole 0.1 ~ 0.6mg/L, dodecyl sodium sulfate 0.05 ~ 0.2g/L, CNT 0.5 ~ 1.5g/ L。
The electroplate liquid that automobile terminal stannum copper carbon nanotubes composite coatings the most according to claim 3 uses, it is characterised in that Formula is as follows: stannous sulfate 30g/L, copper sulfate 3g/L, citric acid 50g/L, tartaric acid 35g/L, 98% sulphuric acid 100mL/L, 2- Mercaptobenzimidazole 0.4mg/L, dodecyl sodium sulfate 0.1 g/L, CNT 1 g/L.
5. use the electroplate liquid described in claim 3 to form the automobile terminal stannum copper CNT Composite Coatings described in claim 1 The electro-plating method of layer, it is characterised in that step is as follows:
(1) in clean coating bath, add deionized water, be slowly added into 98% sulphuric acid, after solution is cooled to 25 ~ 35 DEG C, adds sulphuric acid Stannous, copper sulfate, citric acid, tartaric acid and 2-mercaptobenzimidazole, and constantly it is stirred to dissolve wiring solution-forming A;
(2) dodecyl sodium sulfate and CNT are added in deionized water, within 8 ~ 15 minutes, be made into molten by ultrasound wave dispersion Liquid B;
(3) solution B is added in solution A, hang tin anode and corrugated type electrolytic iron minus plate, and low through 1.5 ~ 2.5 hours Current electroanalysis processes, and obtains electroplate liquid, and the concentration of the most each component is: stannous sulfate 25 ~ 35g/L, copper sulfate 1 ~ 5g/L, Citric acid 45 ~ 55g/L, tartaric acid 30 ~ 40g/L, 98% sulphuric acid 95 ~ 105mL/L, 2-mercaptobenzimidazole 0.1 ~ 0.6mg/L, ten Dialkyl sulfonates 0.05 ~ 0.2g/L, CNT 0.5 ~ 1.5g/L;
(4) automobile terminal through 3 ~ 8 minutes ultrasonic oil removal, 10% add cylinder, at the electricity of 25 DEG C after sulfuric acid activated 3 ~ 8 seconds In plating solution, cathode-current density 3A/dm2And electroplate 8 ~ 12 minutes under conditions of rolling speed 8 revs/min.
The electro-plating method of automobile terminal stannum copper carbon nanotubes composite coatings the most according to claim 5, it is characterised in that: institute State the cumulative volume of the deionized water of the volume of deionized water in the volume+step (2) of deionized water in step (1)=required.
The electro-plating method of automobile terminal stannum copper carbon nanotubes composite coatings the most according to claim 5, it is characterised in that: institute State deionized water in the volume+step (2) of deionized water in step (1) volume < during the cumulative volume of required deionized water, In step (3) solution B is added in solution A, add deionized water the most again to volume required.
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CN103022449A (en) * 2012-12-21 2013-04-03 湘潭大学 Carbon nano tube-Sn-M alloy cathode material and preparation method thereof
CN103022418A (en) * 2012-12-21 2013-04-03 湘潭大学 Carbon nano tube enhanced tin-copper-nickel alloy cathode and preparation method thereof
CN103227369A (en) * 2012-01-26 2013-07-31 三菱综合材料株式会社 Tin-plated copper-alloy material for terminal and method for producing the same
WO2015012275A1 (en) * 2013-07-22 2015-01-29 独立行政法人産業技術総合研究所 Cnt metal composite material, and method for producing same

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
WO2012091139A1 (en) * 2010-12-28 2012-07-05 独立行政法人産業技術総合研究所 Carbon nanotube metal composite material and production method for same
CN103227369A (en) * 2012-01-26 2013-07-31 三菱综合材料株式会社 Tin-plated copper-alloy material for terminal and method for producing the same
CN103022449A (en) * 2012-12-21 2013-04-03 湘潭大学 Carbon nano tube-Sn-M alloy cathode material and preparation method thereof
CN103022418A (en) * 2012-12-21 2013-04-03 湘潭大学 Carbon nano tube enhanced tin-copper-nickel alloy cathode and preparation method thereof
WO2015012275A1 (en) * 2013-07-22 2015-01-29 独立行政法人産業技術総合研究所 Cnt metal composite material, and method for producing same

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