CN107460527A - A kind of nano aluminum nitride composite plating solution and electro-plating method - Google Patents
A kind of nano aluminum nitride composite plating solution and electro-plating method Download PDFInfo
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- CN107460527A CN107460527A CN201710736671.8A CN201710736671A CN107460527A CN 107460527 A CN107460527 A CN 107460527A CN 201710736671 A CN201710736671 A CN 201710736671A CN 107460527 A CN107460527 A CN 107460527A
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- 238000007747 plating Methods 0.000 title claims abstract description 89
- 239000002131 composite material Substances 0.000 title claims abstract description 61
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 35
- 238000009713 electroplating Methods 0.000 title claims abstract description 30
- 239000002270 dispersing agent Substances 0.000 claims abstract description 12
- 238000002203 pretreatment Methods 0.000 claims abstract description 7
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical compound CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 8
- MORMPWNLQJTSOT-UHFFFAOYSA-L disodium;4-dodecyl-2-(4-sulfonatophenoxy)benzenesulfonate Chemical compound [Na+].[Na+].CCCCCCCCCCCCC1=CC=C(S([O-])(=O)=O)C(OC=2C=CC(=CC=2)S([O-])(=O)=O)=C1 MORMPWNLQJTSOT-UHFFFAOYSA-L 0.000 claims description 7
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 4
- 125000000129 anionic group Chemical group 0.000 claims description 4
- -1 neopelex Chemical compound 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 238000009792 diffusion process Methods 0.000 claims 1
- 238000000576 coating method Methods 0.000 abstract description 23
- 239000011248 coating agent Substances 0.000 abstract description 21
- HTKFORQRBXIQHD-UHFFFAOYSA-N allylthiourea Chemical compound NC(=S)NCC=C HTKFORQRBXIQHD-UHFFFAOYSA-N 0.000 abstract description 17
- 229960001748 allylthiourea Drugs 0.000 abstract description 17
- PEYVWSJAZONVQK-UHFFFAOYSA-N hydroperoxy(oxo)borane Chemical compound OOB=O PEYVWSJAZONVQK-UHFFFAOYSA-N 0.000 abstract description 17
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 abstract description 17
- 239000001509 sodium citrate Substances 0.000 abstract description 17
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 abstract description 16
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 abstract description 16
- 239000007788 liquid Substances 0.000 abstract description 14
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 abstract description 10
- 230000035939 shock Effects 0.000 abstract description 8
- 238000005260 corrosion Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 6
- 230000007797 corrosion Effects 0.000 abstract description 5
- 239000011159 matrix material Substances 0.000 abstract description 4
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 description 16
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 description 16
- 239000000243 solution Substances 0.000 description 16
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 14
- 206010001497 Agitation Diseases 0.000 description 10
- 238000013019 agitation Methods 0.000 description 10
- 239000000758 substrate Substances 0.000 description 9
- 239000007864 aqueous solution Substances 0.000 description 8
- 239000008236 heating water Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 238000010907 mechanical stirring Methods 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 229910052759 nickel Inorganic materials 0.000 description 6
- 238000012360 testing method Methods 0.000 description 5
- 230000033228 biological regulation Effects 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 238000002604 ultrasonography Methods 0.000 description 4
- 229910017083 AlN Inorganic materials 0.000 description 3
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 description 3
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- 239000002105 nanoparticle Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 244000137852 Petrea volubilis Species 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 229910052804 chromium Inorganic materials 0.000 description 2
- 239000011651 chromium Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N dodecane Chemical compound CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 241000080590 Niso Species 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- CXKCTMHTOKXKQT-UHFFFAOYSA-N cadmium oxide Inorganic materials [Cd]=O CXKCTMHTOKXKQT-UHFFFAOYSA-N 0.000 description 1
- CFEAAQFZALKQPA-UHFFFAOYSA-N cadmium(2+);oxygen(2-) Chemical compound [O-2].[Cd+2] CFEAAQFZALKQPA-UHFFFAOYSA-N 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000008151 electrolyte solution Substances 0.000 description 1
- 229910001651 emery Inorganic materials 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 229910021421 monocrystalline silicon Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 125000001400 nonyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- GCCVBRCGRJWMDX-UHFFFAOYSA-N phenoxybenzene;sodium Chemical compound [Na].C=1C=CC=CC=1OC1=CC=CC=C1 GCCVBRCGRJWMDX-UHFFFAOYSA-N 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/10—Agitating of electrolytes; Moving of racks
-
- 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
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating And Plating Baths Therefor (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The present invention, which provides a kind of nano aluminum nitride composite plating solution and electro-plating method, its electroplate liquid, mainly to be included：NiSO4·6H2O、Ni2Cl·6H2O, KCl, sodium citrate, Allyl thiourea, HBO3, nano aluminum nitride, composite dispersing agent.Its electro-plating method mainly includes the following steps that：（1）Prepare composite plating solution；（2）Plating piece pre-treatment；（3）Composite plating solution is poured into electrolytic cell, and determines composite plating process parameter, carries out composite plating；（4）Composite plating is completed, plating piece is carried out and processes in next step.Coating stability prepared by nano aluminum nitride composite plating solution and electro-plating method provided by the invention is good, and strong with matrix material adhesion, coating is closely uniform, wear-resisting, corrosion-resistant, thermal shock resistance is good, has good High temperature and insulating heat conductive performance.Electroplating technology of the present invention is simple, and gained coating performance is excellent, and adhesion is good, easily operated popularization.
Description
Technical field
The present invention relates to electrochemistry and field of metal surface treatment technology, and in particular to a kind of nano aluminum nitride composite plating
Liquid and electro-plating method.
Background technology
Composite Coatings refer to make metal and insoluble non-metal solid with electrochemistry or chemical method in electrolyte solution
The technique for the composite layer that grain (or other metal particles) is co-deposited and obtains.Composite Coatings plating turns into nearly many decades people
The much-talked-about topic studied, its commercial Application track to 1970.For a long time, composite plating work is studied to be concentrated mainly on
Anti-corrosion, wear-resisting, self-lubricating and the research of dispersion-strengthened coating.In recent years, it is nanocrystalline, nanometer is multiple with the development of nanosecond science and technology
Close electro-deposition and also climb up plating stage.
Due to the compound denominator crossed with dispersed particle and parent metal, adding the particle of different qualities can obtain
The various composite deposite of property.The nano-composite plate studied at present is concentrated mainly on following several types：(1) high rigidity,
Nanometer antiwear coating；(2) high-temperature oxidation resistant, high-temperature wear-resistant nanometer composite deposite；(3) have high photocatalytic activity nano combined
Coating；(4) there is high electro catalytic activity nano-deposit；(5) corrosion resistant nano-composite deposit.These coated metal matrixes are most
Based on Ni-based, chromium base, but due to chromium strong toxicity, pollution is big, progressively by Ni-based substitution.Its nano particle is according to coating need
Ask from indissoluble and chemically stable nano-particles such as alundum (Al2O3), carborundum, diamond, cadmium oxide, titanium oxide.
Nano aluminum nitride is a kind of DLC nitride, is High-heat-conductiviinsulation insulation material best at present, and highest can be stablized
To 2200 DEG C, thermal coefficient of expansion is low, close with monocrystalline silicon, and its room temperature strength is high, and intensity is slower with the rise decline of temperature, is
A kind of resistance is high, the heat shock resistance material that material under high temperature intensity is big, hardness is high, interface compatibility is good, nontoxic.
With development in science and technology, in order to adapt to various intensive work environment, usually to equipment part or instrument in instrument and equipment
Device integrally plates the high-temperature wear resistant coating for meeting various particular/special requirements, but how to ensure the insulation of metal parts under hot conditions
Property, heat conductivility, usually as the difficult point in precision instrument, and many materials thermal coefficient of expansion is big, and thermal shock resistance is inadequate,
Its service life is had a greatly reduced quality, influence the performance of instrument or equipment, also increase the operating cost of instrument or equipment.
The content of the invention
It is common with nickel using aluminium nitride the invention provides a kind of nano aluminum nitride composite plating solution for prior art
Matrix surface is deposited on, it is a kind of big, wear-resisting, corrosion-resistant, heat shock resistance without chrome plating with hardness to obtain.
Present invention also offers the electro-plating method of the nano aluminum nitride composite plating solution, and its electro-plating method technique is simple,
Easily promote, the binding force of cladding material of acquisition is good, function admirable.
A kind of nano aluminum nitride composite plating solution that the present invention uses, its electroplate liquid include following components：
Further, its key component is preferably：
Further, the composite dispersing agent be include 60~90 ω t% anionic dispersing agents and 10~40 ω t% it is non-
The mixture of ionic dispersants.The anionic dispersing agents include lauryl sodium sulfate, neopelex, dodecane
One kind in yl diphenyl ether sodium disulfonate；The non-ionic dispersing agent includes OPEO, Nonyl pheno
One kind in ether, Lauryl Alcohol APEO, Lauryl Alcohol APEO.The particle diameter of the nano aluminum nitride be 30~
60nm。
The nano aluminum nitride composite plating solution, its electro-plating method comprise the following steps：
(1) composite plating solution is prepared；
(2) plating piece pre-treatment；
(3) composite plating solution is poured into electrolytic cell, and determines composite plating process parameter, carry out composite plating；
(4) composite plating is completed, plating piece is carried out and processes in next step.
The composite plating process parameter setting is：
Cathode-current density：1.5~5A/dm2
pH：3.8~4.5
Temperature：30~45 DEG C.
Wherein, cathode-current density is preferably 2~3A/dm2。
Nano aluminum nitride selects purity >=99.5%, specific surface area >=60m in the present invention2/ g, total oxygen≤0.5%
Hexagonal structure aluminium nitride, other bath components Analysis about Selection are pure and above medicine is as raw material., will in the step (1)
Nano aluminum nitride is added in the aqueous solution dissolved with composite dispersing agent, nano dispersion fluid is obtained after shearing is scattered, then according to electricity
The content of each component adds NiSO in plating solution4·6H2O、NiCl2·6H2O, KCl, sodium citrate, Allyl thiourea, HBO3, dissolving
It is standby after ultrasonic disperse after completely.
In the step (2), plating piece pre-treatment includes derusting, oil removing, polish, be polished to and bright luster occur after, with third
After ketone or absolute ethyl alcohol cleaning are clean, dry standby.
In electroplating process, the electroplate liquid is disperseed simultaneously with ultrasound and mechanical agitation or magnetic agitation, prevents from receiving
Rice grain settles, and reaches more preferable dispersion effect, makes nano aluminum nitride as nickel uniform deposition is in matrix surface.
Beneficial effect：
(1) a kind of nano aluminum nitride composite plating solution provided by the invention, using resistance is high, material under high temperature intensity is big,
The nano aluminum nitride that hardness is high, interface compatibility is good, nontoxic can improve the hardness, wear-resisting of coating as nonmetallic phase is not allowed
Performance, decay resistance, high-temperature heat-conductive performance and thermal shock resistance.It is resistance to meanwhile nano aluminum nitride material thermal expansion coefficient is small
Thermal shock ability is strong, can extend the service life of plating piece.
(2) the coating stability that prepared by nano aluminum nitride composite plating solution and electro-plating method provided by the invention is good, with base
Body material adhesion is strong, and coating is closely uniform, wear-resisting, corrosion-resistant, thermal shock resistance is good, has good High temperature and insulating heat conductive
Performance.Electroplating technology of the present invention is simple, and gained coating performance is excellent, and adhesion is good, easily operated popularization.
Embodiment
Technical scheme is further described below by embodiment.
The present invention, which provides a kind of nano aluminum nitride composite plating solution and electro-plating method, its electroplate liquid, mainly to be included：NiSO4·
6H2O、NiCl2·6H2O, KCl, sodium citrate, Allyl thiourea, HBO3, nano aluminum nitride, composite dispersing agent.Its electro-plating method
Mainly include the following steps that：(1) composite plating solution is prepared；(2) plating piece pre-treatment；(3) composite plating solution is poured into electrolytic cell,
And composite plating process parameter is determined, carry out composite plating；(4) composite plating is completed, plating piece is carried out and processes in next step.
It is embodied as：
(1) composite plating solution is prepared
The composite plating solution weighs according to the formula listed by table 1：
Table 1
(2) plating piece pre-treatment
The plating nickel plate that selection purity is more than 99.5% is as anode substrate, it is necessary to the metal plating piece or alloy of plating
Plating piece carries out pre-treatment as cathode base.After plating piece derusting, oil removing, first with 120 mesh, once sand paper or emery wheel are beaten
Mill, then successively with 200 mesh, 400 mesh, 800 mesh sand paper sanding and polishings to after there is bright luster, dirt is rinsed with clear water, then use
After absolute ethyl alcohol wipes several times, dry standby.
(3) composite plating process parameter is set
The composite plating solution prepared in step (1) is poured into electrolytic cell, and heating water bath is incubated to 30~45 DEG C,
Rotating speed is 100~200r/min mechanical agitations, nano-particle in its electroplate liquid is kept scattered, and measure its pH value again.Beat
Ultrasonic device is opened, its supersonic frequency is 200~400kHz, while electroplate liquid is disperseed using mechanical agitation and ultrasound, is made
In electroplating process, nano aluminum nitride is dispersed in nickel coating.Meanwhile ultrasound is used while point spread with mechanical agitation,
Be advantageous to the refinement of nickel coating particle, make in coating crystal grain more tiny close, improve the performance of coating.By cathode base and sun
Pole matrix is put into electrolytic cell, is switched on power, 1.5~5A/dm of cathode-current density2Electroplate 20~60min.In electroplating process,
Its electroplating time thickness of coating according to needed for cathode base is adjusted.
(4) composite plating is completed, carries out the next step processing of plating piece
After the completion of plating, power supply is closed, anode substrate and cathode base is taken out, is dried after cleaning, according to other of plating piece
Performance and customer demand carry out next step processing, and carry out the coating detection of plating piece.
Embodiment 1
Each component content according to the listed formula of table 2 carries out weighing for bath components.
| Title | Content (g/L) | Title | Content (g/L) |
| Nano aluminum nitride | 29 | HBO3 | 20 |
| NiSO4·6H2O | 250 | Sodium citrate | 20 |
| NiCl2·6H2O | 95 | Allyl thiourea | 1.2 |
| KCl | 50 | OPEO | 0.05 |
| Neopelex | 0.1 |
Table 2
The nano aluminum nitride weighed is added to the aqueous solution of neopelex and NPE
In, disperse 15min in 400r/min low speed, then using 2000r/min at a high speed scattered 15min after, add it is load weighted other into
Point：NiSO4·6H2O、NiCl2·6H2O, KCl, sodium citrate, Allyl thiourea, HBO3, after dissolving completely, regulation pH value is
3.8, ultrasonic disperse 5min, standby under 400kHz frequency.The electroplate liquid prepared is added to be provided with mechanical agitation and
In the electroplating bath of ultrasonic device, heating water bath opens mechanical stirring equipment to 30 DEG C, and its rotating speed is arranged to 200r/min, surveys
After determining pH value, cathode base and anode substrate are put into, it is ultrasonic under 200kHz frequencies, and power-on, by average current density
For 1.5A/dm2, 25min is electroplated, closes power supply, cathode base plating is completed, obtains plating piece.
Embodiment 2
Each component content according to the listed formula of table 3 carries out weighing for bath components.
| Title | Content (g/L) | Title | Content (g/L) |
| Nano aluminum nitride | 25 | HBO3 | 28 |
| NiSO4·6H2O | 330 | Sodium citrate | 30 |
| NiCl2·6H2O | 50 | Allyl thiourea | 1.1 |
| KCl | 95 | NPE | 0.1 |
| Neopelex | 0.5 |
Table 3
The nano aluminum nitride weighed is added to the aqueous solution of neopelex and NPE
In, disperse 10min in 500r/min low speed, then using 2000r/min at a high speed scattered 15min after, add it is load weighted other into
Point：NiSO4·6H2O、NiCl2·6H2O, KCl, sodium citrate, Allyl thiourea, HBO3, after dissolving completely, regulation pH value is
4.0, ultrasonic disperse 5min, standby under 300kHz frequency.The electroplate liquid prepared is added to be provided with mechanical agitation and
In the electroplating bath of ultrasonic device, heating water bath opens mechanical stirring equipment to 40 DEG C, and its rotating speed is arranged to 180r/min, surveys
After determining pH value, cathode base and anode substrate are put into, it is ultrasonic under 200kHz frequencies, and power-on, by average current density
For 1.5A/dm2, 50min is electroplated, closes power supply, cathode base plating is completed, obtains plating piece.
Embodiment 3
Each component content according to the listed formula of table 4 carries out weighing for bath components.
| Title | Content (g/L) | Title | Content (g/L) |
| Nano aluminum nitride | 22 | HBO3 | 26 |
| NiSO4·6H2O | 320 | Sodium citrate | 28 |
| NiCl2·6H2O | 60 | Allyl thiourea | 0.8 |
| KCl | 85 | NPE | 0.2 |
| Lauryl sodium sulfate | 1.5 |
Table 4
The nano aluminum nitride weighed is added to the aqueous solution of lauryl sodium sulfate and Lauryl Alcohol APEO
In, disperse 10min in 500r/min low speed, then using 2200r/min at a high speed scattered 10min after, add it is load weighted other into
Point：NiSO4·6H2O、NiCl2·6H2O, KCl, sodium citrate, Allyl thiourea, HBO3, after dissolving completely, regulation pH value is
3.5, ultrasonic disperse 3min, standby under 500kHz frequency.The electroplate liquid prepared is added to be provided with mechanical agitation and
In the electroplating bath of ultrasonic device, heating water bath opens mechanical stirring equipment to 55 DEG C, and its rotating speed is arranged to 100r/min, surveys
After determining pH value, cathode base and anode substrate are put into, it is ultrasonic under 400kHz frequencies, and power-on, by average current density
For 2A/dm2, 25min is electroplated, closes power supply, cathode base plating is completed, obtains plating piece.
Embodiment 4
Each component content according to the listed formula of table 5 carries out weighing for bath components.
| Title | Content (g/L) | Title | Content (g/L) |
| Nano aluminum nitride | 16 | HBO3 | 24 |
| NiSO4·6H2O | 300 | Sodium citrate | 24 |
| NiCl2·6H2O | 75 | Allyl thiourea | 0.9 |
| KCl | 70 | Lauryl Alcohol APEO | 0.2 |
| Lauryl sodium sulfate | 1 |
Table 4
The nano aluminum nitride weighed is added to the aqueous solution of lauryl sodium sulfate and Lauryl Alcohol APEO
In, disperse 15min in 400r/min low speed, then using 2200r/min at a high speed scattered 10min after, add it is load weighted other into
Point：NiSO4·6H2O、NiCl2·6H2O, KCl, sodium citrate, Allyl thiourea, HBO3, after dissolving completely, regulation pH value is 4,
Ultrasonic disperse 4min, standby under 400kHz frequency.The electroplate liquid prepared is added to and is provided with mechanical agitation and ultrasound
In the electroplating bath of equipment, heating water bath opens mechanical stirring equipment to 55 DEG C, and its rotating speed is arranged to 150r/min, determines pH
After value, cathode base and anode substrate are put into, it is ultrasonic under 400kHz frequencies, and power-on, it is 2A/ by average current density
dm2, 50min is electroplated, closes power supply, cathode base plating is completed, obtains plating piece.
Embodiment 5
Each component content according to the listed formula of table 6 carries out weighing for bath components.
| Title | Content (g/L) | Title | Content (g/L) |
| Nano aluminum nitride | 14 | HBO3 | 22 |
| NiSO4·6H2O | 280 | Sodium citrate | 22 |
| NiCl2·6H2O | 60 | Allyl thiourea | 1.0 |
| KCl | 90 | Lauryl Alcohol APEO | 0.05 |
| Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate | 0.3 |
Table 6
The nano aluminum nitride weighed is added to disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate and OPEO
In the aqueous solution, disperse 15min in 40r/min low speed, then using 2200r/min at a high speed scattered 10min after, add it is load weighted its
His composition：NiSO4·6H2O、NiCl2·6H2O, KCl, sodium citrate, Allyl thiourea, HBO3, after dissolving completely, adjust pH value
For 4.5, ultrasonic disperse 4min, standby under 400kHz frequency.The electroplate liquid prepared is added to and is provided with mechanical agitation
In the electroplating bath of ultrasonic device, heating water bath opens mechanical stirring equipment to 50 DEG C, and its rotating speed is arranged to 150r/min,
After determining pH value, cathode base and anode substrate are put into, it is ultrasonic under 300kHz frequencies, and power-on, average current is close
Spend for 3A/dm2, 25min is electroplated, closes power supply, cathode base plating is completed, obtains plating piece.
Embodiment 6
Each component content according to the listed formula of table 7 carries out weighing for bath components.
| Title | Content (g/L) | Title | Content (g/L) |
| Nano aluminum nitride | 10 | HBO3 | 20 |
| NiSO4·6H2O | 260 | Sodium citrate | 24 |
| NiCl2·6H2O | 60 | Allyl thiourea | 1.0 |
| KCl | 90 | OPEO | 0.05 |
| Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate | 0.3 |
Table 7
The nano aluminum nitride weighed is added to disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate and OPEO
In the aqueous solution, disperse 15min in 400r/min low speed, then using 2200r/min at a high speed scattered 10min after, add load weighted
Other compositions：NiSO4·6H2O、NiCl2·6H2O, KCl, sodium citrate, Allyl thiourea, HBO3, after dissolving completely, adjust pH
It is worth for 4.5, ultrasonic disperse 4min, standby under 400kHz frequency.The electroplate liquid prepared is added to and is provided with machinery and stirs
In the electroplating bath for mixing and stirring ultrasonic device, heating water bath opens mechanical stirring equipment to 45 DEG C, and its rotating speed is arranged to 200r/
Min, after determining pH value, cathode base and anode substrate are put into, it is ultrasonic under 300kHz frequencies, and power-on, by average electricity
Current density is 4A/dm2, 30min is electroplated, closes power supply, cathode base plating is completed, obtains plating piece.
Comparative example：
Each component content according to the listed formula of table 8 carries out weighing for bath components.
| Title | Content (g/L) | Title | Content (g/L) |
| NiSO4·6H2O | 320 | HBO3 | 26 |
| NiCl2·6H2O | 60 | Sodium citrate | 28 |
| KCl | 85 | Allyl thiourea | 0.8 |
| Disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate | 1.5 | OPEO | 0.2 |
Table 8
The nano aluminum nitride weighed is added to disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate and OPEO
In the aqueous solution, disperse 15min in 400r/min low speed, then using 2200r/min at a high speed scattered 10min after, add load weighted
Other compositions：NiSO4·6H2O、NiCl2·6H2O, KCl, sodium citrate, Allyl thiourea, HBO3, after dissolving completely, adjust pH
It is worth for 4.5, ultrasonic disperse 4min, standby under 400kHz frequency.The electroplate liquid prepared is added to and is provided with machinery and stirs
In the electroplating bath for mixing and stirring ultrasonic device, heating water bath opens mechanical stirring equipment to 45 DEG C, and its rotating speed is arranged to 200r/
Min, after determining pH value, cathode base and anode substrate are put into, it is ultrasonic under 300kHz frequencies, and power-on, by average electricity
Current density is 4A/dm2, 30min is electroplated, closes power supply, cathode base plating is completed, obtains plating piece.
After plating terminates, with visual method examine coating have it is pin-free, come off, play knurl, burn phenomena such as, and carry out coating
Porosity test, hardness test, salt spray test, wear-resisting experiment and hot jolt ramming are tested.
Table 9 is test result.
Table 9
From test result table, the porosity of nickel coating is contrasted, hardness, salt spray resistance, wear-resisting and hot jolt ramming are tested, addition is received
The composite deposite of rice aluminium nitride is substantially better than the former, has more preferable wear resistant corrosion resistant and thermal shock resistance.
The present invention is not limited to above-mentioned preferred forms, and anyone can show that other are various under the enlightenment of the present invention
The product of form, however, make any change in its shape or structure, it is every that there is skill identical or similar to the present application
Art scheme, is within the scope of the present invention.
Claims (8)
- A kind of 1. nano aluminum nitride composite plating solution, it is characterised in that：The composite plating solution key component includes：
- A kind of 2. nano aluminum nitride composite plating solution according to claim 1, it is characterised in that：The composite plating solution master Component is wanted to include：
- A kind of 3. nano aluminum nitride composite plating solution according to claim 1 or 2, it is characterised in that：The composite diffusion Agent is the mixture of the anionic dispersing agents and 10~40 ω t% non-ionic dispersing agents that include 60~90 ω t%.
- A kind of 4. nano aluminum nitride composite plating solution according to claim 3, it is characterised in that：The anionic dispersing agents Including one kind in lauryl sodium sulfate, neopelex, disodium 4-dodecyl-2,4 '-oxydibenzenesulfonate；The nonionic Dispersant includes OPEO, NPE, Lauryl Alcohol APEO, Lauryl Alcohol polyoxy second One kind in alkene ether.
- 5. a kind of nano aluminum nitride composite plating solution according to claim 1 or 2 and electro-plating method, it is characterised in that：Institute The particle diameter for stating nano aluminum nitride is 30~60nm.
- A kind of 6. electro-plating method of nano aluminum nitride composite plating solution according to claim 1 or 2, it is characterised in that：Institute Electro-plating method is stated to comprise the following steps：(1) composite plating solution is prepared；(2) plating piece pre-treatment；(3) composite plating solution is poured into electrolytic cell, and determines composite plating process parameter, carry out composite plating；(4) composite plating is completed, plating piece is carried out and processes in next step.
- A kind of 7. electro-plating method of nano aluminum nitride composite plating solution according to claim 6, it is characterised in that：The step Suddenly composite plating process parameter setting is in (3)：Cathode-current density：1.5~5A/dm2pH：3.8~4.5Temperature：30~45 DEG C.
- A kind of 8. electro-plating method of nano aluminum nitride composite plating solution according to claim 7, it is characterised in that：The step Suddenly cathode-current density is in (3)：2~3A/dm2。
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