CN111893464A - Preparation method for plating Ni-P film on surface of aluminum alloy substrate - Google Patents
Preparation method for plating Ni-P film on surface of aluminum alloy substrate Download PDFInfo
- Publication number
- CN111893464A CN111893464A CN202010730674.2A CN202010730674A CN111893464A CN 111893464 A CN111893464 A CN 111893464A CN 202010730674 A CN202010730674 A CN 202010730674A CN 111893464 A CN111893464 A CN 111893464A
- Authority
- CN
- China
- Prior art keywords
- nickel
- aluminum alloy
- plating
- acid
- film
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 238000007747 plating Methods 0.000 title claims abstract description 56
- 229910000838 Al alloy Inorganic materials 0.000 title claims abstract description 43
- 239000000758 substrate Substances 0.000 title claims abstract description 29
- 229910018104 Ni-P Inorganic materials 0.000 title claims abstract description 23
- 229910018536 Ni—P Inorganic materials 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 93
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 46
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000005530 etching Methods 0.000 claims abstract description 15
- 238000004140 cleaning Methods 0.000 claims abstract description 12
- 239000002253 acid Substances 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 11
- 238000004506 ultrasonic cleaning Methods 0.000 claims abstract description 10
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 8
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 8
- 230000003213 activating effect Effects 0.000 claims abstract description 7
- 239000000463 material Substances 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 12
- 230000035484 reaction time Effects 0.000 claims description 11
- 229910001868 water Inorganic materials 0.000 claims description 11
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 10
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000002386 leaching Methods 0.000 claims description 8
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 8
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 6
- 239000004327 boric acid Substances 0.000 claims description 6
- 238000005282 brightening Methods 0.000 claims description 6
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 6
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 6
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 6
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 6
- JVTAAEKCZFNVCJ-REOHCLBHSA-N L-lactic acid Chemical compound C[C@H](O)C(O)=O JVTAAEKCZFNVCJ-REOHCLBHSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 claims description 4
- 229940040526 anhydrous sodium acetate Drugs 0.000 claims description 4
- 238000011068 loading method Methods 0.000 claims description 4
- 239000011775 sodium fluoride Substances 0.000 claims description 4
- 235000013024 sodium fluoride Nutrition 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 244000137852 Petrea volubilis Species 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 238000007781 pre-processing Methods 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 239000001488 sodium phosphate Substances 0.000 claims description 2
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 2
- 230000002378 acidificating effect Effects 0.000 abstract description 9
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 abstract description 8
- 238000007598 dipping method Methods 0.000 abstract description 5
- 238000005498 polishing Methods 0.000 abstract description 5
- 239000000956 alloy Substances 0.000 abstract description 3
- 230000007547 defect Effects 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 3
- 238000002791 soaking Methods 0.000 abstract description 3
- 239000002585 base Substances 0.000 description 24
- 230000004913 activation Effects 0.000 description 11
- 238000000576 coating method Methods 0.000 description 9
- 239000011159 matrix material Substances 0.000 description 7
- 239000003513 alkali Substances 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 238000007654 immersion Methods 0.000 description 6
- 238000005406 washing Methods 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 5
- 239000008139 complexing agent Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 238000000227 grinding Methods 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000006172 buffering agent Substances 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 239000003638 chemical reducing agent Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000004310 lactic acid Substances 0.000 description 2
- 235000014655 lactic acid Nutrition 0.000 description 2
- 150000002815 nickel Chemical class 0.000 description 2
- 229910052755 nonmetal Inorganic materials 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000003755 preservative agent Substances 0.000 description 2
- 230000002335 preservative effect Effects 0.000 description 2
- -1 salt nickel sulfate Chemical class 0.000 description 2
- 238000012876 topography Methods 0.000 description 2
- 229910000406 trisodium phosphate Inorganic materials 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000000724 energy-dispersive X-ray spectrum Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/31—Coating with metals
- C23C18/32—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron
- C23C18/34—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents
- C23C18/36—Coating with nickel, cobalt or mixtures thereof with phosphorus or boron using reducing agents using hypophosphites
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1806—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by mechanical pretreatment, e.g. grinding, sanding
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/16—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by reduction or substitution, e.g. electroless plating
- C23C18/18—Pretreatment of the material to be coated
- C23C18/1803—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces
- C23C18/1824—Pretreatment of the material to be coated of metallic material surfaces or of a non-specific material surfaces by chemical pretreatment
- C23C18/1837—Multistep pretreatment
- C23C18/1844—Multistep pretreatment with use of organic or inorganic compounds other than metals, first
Landscapes
- Chemical & Material Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemically Coating (AREA)
Abstract
The invention relates to a preparation method for plating a Ni-P film on the surface of an aluminum alloy substrate. The defect that a firm amorphous thick nickel-phosphorus film layer cannot be formed on the surface of an aluminum alloy substrate in the prior art is overcome. The method comprises the steps of conventionally polishing the aluminum alloy; ultrasonic cleaning; oil removal and alkaline etching; emitting light; activating and soaking nickel; alkaline preplating; acid nickel plating; cleaning; and (5) drying. The invention carries out chemical nickel dipping treatment after the aluminum alloy material is pretreated and is bright dipping by nitric acid and hydrofluoric acid, and can form a firm nickel-phosphorus film layer by the methods of alkaline preplating and acidic chemical nickel plating, and the plating speed reaches 11 mu m/h. Completely meets the technical requirement of plating a thick nickel-phosphorus film on the surface of the aluminum alloy.
Description
Technical Field
The invention belongs to the technical field of preparation of aluminum-based composite material coating films, and particularly relates to a preparation method of a Ni-P coating film on the surface of an aluminum alloy substrate.
Background
Aluminium alloy surfaceThe coating is much more difficult than other metal coatings because aluminum has strong affinity with oxygen, an oxide film is easily generated on the surface, and the bonding force with the coating is poor. The traditional film plating method comprises an electroplating method and a direct chemical plating method, and the two methods often have the phenomena of weak combination between an aluminum alloy substrate and a plating layer, and bubbling and even shedding of the plating layer. The reason is as follows: the standard electrode potential of aluminum is very negative
The metal ions with the correct point positions are easy to generate displacement reaction in the plating solution to generate a loose layer (contact layer), so that the bonding force between the plating layer and the aluminum matrix is reduced; secondly, the difference between the surface expansion coefficient of the aluminum and the expansion coefficient of most metal coatings is large, hydrogen is often occluded between the aluminum substrate and the coatings, and the bonding force between the coatings and the substrate is often reduced due to the defects of local pores or pores in the aluminum alloy substrate; the key point is to obtain an amorphous thick nickel-phosphorus coating with strong bonding force and excellent performance on the surface of the aluminum alloy before plating.
Disclosure of Invention
The invention aims to provide a preparation method for plating a thick Ni-P film on the surface of an aluminum alloy substrate, which overcomes the defect that a firm amorphous thick nickel-phosphorus film layer cannot be formed on the surface of the aluminum alloy substrate in the prior art.
In order to solve the technical problem, the invention provides a preparation method for plating a Ni-P film on the surface of an aluminum alloy substrate, which comprises the following steps:
firstly, preprocessing an aluminum alloy base material: including sanding, ultrasonic cleaning, degreasing and alkaline etching.
And step two, performing light-emitting treatment on the aluminum alloy base material by using a solution prepared from nitric acid, hydrofluoric acid and water.
And step three, carrying out activation nickel immersion treatment on the aluminum alloy base material by using nickel sulfate, hydrofluoric acid and boric acid solution.
Step four, carrying out alkaline nickel preplating treatment on the aluminum alloy base material by using nickel sulfate, sodium hypophosphite and sodium pyrophosphate, wherein the solution ratio is as follows: nickel sulfate 25 &30g/L, 25-30 g/L sodium hypophosphite, 50-60 g/L sodium pyrophosphate, and NH3·H2Adjusting the pH value to about 10 by O, controlling the reaction temperature to 45 ℃ and controlling the reaction time to 5 min.
Step five, performing acid chemical nickel plating treatment on the aluminum alloy base material: 25-30 g/L nickel sulfate, 30-35 g/L sodium hypophosphite, 15-20 mL/L lactic acid, 5-10 g/L citric acid, 15-20 g/L anhydrous sodium acetate, 1g/L sodium fluoride, and NH3·H2Adjusting the pH value to 4.5-4.6 by O, and the loading capacity is about 1dm2and/L, the reaction temperature is 88 ℃, and the plating solution is changed every 1 hour.
In the first step, the types of the used sand paper are as follows: 120#, 240#, 600#, 1000#, 1500 #; the solvents for ultrasonic cleaning were: absolute ethyl alcohol, and the cleaning time is 10 min; solution proportioning for oil removal and alkaline etching: 20g/L of sodium carbonate, 30g/L of sodium phosphate, 5g/L of sodium hydroxide, 50 ℃ of reaction temperature and 3-5 min of reaction time.
In the second step, the used brightening liquid is: nitric acid, hydrofluoric acid and water in a ratio of 3:1:1, wherein the reaction time is 3-5 s.
In the third step, the proportion of the activating nickel-leaching solution is as follows: 25-30 g/L of nickel sulfate, 90-100 mL/L of hydrofluoric acid and 30-40 g/L of boric acid, and the reaction time is 5min at room temperature.
Cleaning steps are added between the steps, and in the cleaning steps, deionized water is adopted to clean the aluminum alloy base material, and then the next step operation is carried out.
Compared with the prior art, the invention has the advantages that:
the invention carries out chemical nickel dipping treatment after the aluminum alloy material is pretreated and is bright dipping by nitric acid and hydrofluoric acid, and can form a firm nickel-phosphorus film layer by the methods of alkaline preplating and acidic chemical nickel plating, and the plating speed reaches 11 mu m/h. Completely meets the technical requirement of plating a thick nickel-phosphorus film on the surface of the aluminum alloy.
Drawings
FIG. 1 is an SEM image of Ni-P film thickness of 7h, 11h, 12h after chemical acidic nickel plating by activation nickel immersion pretreatment;
FIG. 2 is SEM images of the surface of a 12h Ni-P film layer of chemical acid nickel plating after activation and nickel immersion pretreatment, wherein a and b are respectively surface topography images of two groups of matrixes, and the lower right corner of the image is a 100 mu m scale;
FIG. 3 is an XRD diffractogram of a 12h Ni-P film layer of electroless acidic nickel plating after activation pretreatment;
FIG. 4 is an EDS energy spectrum of a 12h Ni-P film coated with electroless acidic nickel after pretreatment by activation.
Detailed Description
The invention is explained in more detail below with reference to specific embodiments and the drawing.
The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.
Example 1:
a preparation method for plating a Ni-P film on the surface of an aluminum alloy substrate specifically comprises the following steps:
aluminum alloy conventional grinding → ultrasonic cleaning → oil removal, alkaline etching → light extraction → activated nickel immersion → alkaline pre-plating → acid nickel plating → cleaning → drying.
(1) Matrix pretreatment: polishing, ultrasonic cleaning, oil removal and alkaline etching. Aluminum alloy No. 120, No. 240, No. 600, No. 1000 and No. 1500 which are 10mm multiplied by 3mm are sanded, and then are put into absolute ethyl alcohol solution for ultrasonic cleaning for 10min, so that impurities, oil stains and the like carried by the surface of the material due to polishing are removed. According to NaCO3Is 20g/L, Na3PO430g/L and 5g/L NaOH, preparing an alkali etching and oil removing solution, wherein the reaction temperature is 50 ℃ and the reaction time is 3 min.
(2) Light emission: preparation of HNO3:HF:H2O is 3:1: 1. And (3) clamping the base material subjected to oil removal and alkaline etching by using tweezers, quickly putting the base material into a brightening solution for brightening, immediately taking out the base material after the surface of the base material is whitened for about 3-5 s, and washing the base material by using deionized water after the base material is taken out by using the tweezers. The light emission can remove certain metal or nonmetal impurities which can not be removed in the oil removal and alkali corrosion processes on the surface of the aluminum alloy, and simultaneously remove black corrosive substances generated in the alkali corrosion and oil removal processes, so that the matrix is brighter, and simultaneously, the matrix is activatedThe binding force is improved.
(3) Activating and soaking nickel: preparing 100mL of activation nickel leaching solution into a 150mL plastic beaker by using deionized water according to the concentration ratio of 30g/L of nickel sulfate, 90mL/L of hydrofluoric acid and 40g/L of boric acid, cleaning the bright substrate material, and placing the substrate material into the activation nickel leaching solution, wherein the reaction time is 5min at room temperature. And taking out the substrate by using tweezers, and then washing the substrate by using deionized water, wherein the surface of the substrate is grayish white.
(4) Alkaline nickel preplating: preparing 100mL of alkaline nickel pre-plating solution by deionized water according to the concentration ratio of 25g/L of nickel sulfate, 25g/L of sodium hypophosphite and 50g/L of sodium pyrophosphate, and using NH3·H2Adjusting the pH value to 10, putting the base material subjected to the activation nickel leaching treatment into a beaker filled with an alkaline nickel pre-plating solution, putting the beaker into a constant-temperature water bath kettle at 45 ℃, performing alkaline nickel pre-plating treatment for 5min, taking out the base material with tweezers, and then washing the base material with deionized water.
(5) Acid chemical nickel plating: according to the concentration proportion of 25g/L of main salt nickel sulfate, 30g/L of reducing agent sodium hypophosphite, 20mL/L of complexing agent lactic acid, 10g/L of complexing agent citric acid, 15g/L of buffering agent anhydrous sodium acetate and 1g/L of accelerator sodium fluoride, the prepared loading capacity (the ratio of the surface area of a workpiece immersed in the plating solution to the volume of the plating solution) is about 1dm2Acid nickel plating solution of/L, using NH3·H2O adjusted pH 4.5. The basic material which is subjected to alkaline pre-nickel plating is washed clean by deionized water and then quickly placed into a small beaker filled with acidic nickel plating solution, the mouth of the beaker is wrapped by a preservative film and placed into a constant-temperature water bath kettle at 88 ℃ for reaction for 7 hours, and the acidic plating solution is changed every 1 hour.
Example 2:
a preparation method for plating a Ni-P film on the surface of an aluminum alloy substrate specifically comprises the following steps:
aluminum alloy conventional grinding → ultrasonic cleaning → oil removal, alkaline etching → light extraction → activated nickel immersion → alkaline pre-plating → acid nickel plating → cleaning → drying.
(1) Matrix pretreatment: polishing, ultrasonic cleaning, oil removal and alkaline etching. Grinding aluminum alloy No. 120, No. 240, No. 600, No. 1000 and No. 1500 with the thickness of 10mm multiplied by 3mm, and then adding absolute ethyl alcoholUltrasonic cleaning in the solution for 10min to remove impurities, oil stains and the like carried by the surface of the material due to polishing. According to NaCO3Is 20g/L, Na3PO430g/L and 5g/L NaOH, preparing an alkali etching and oil removing solution, and reacting at 50 ℃ for 5 min.
(2) Light emission: preparation of HNO3:HF:H2O is 3:1: 1. Clamping the base material subjected to oil removal and alkaline etching by using tweezers, quickly putting the base material into a brightening solution for brightening, immediately taking out the base material after the surface of the base material is whitened for about 3s, and then taking out the base material by using the tweezers and then washing the base material by using deionized water. The bright dipping can remove some metal or non-metal impurities on the surface of the aluminum alloy which can not be removed in the oil and alkali etching processes, and simultaneously remove black corrosive substances generated in the alkali etching and oil removing processes, so that the matrix is brighter, and simultaneously, the matrix is activated to improve the binding force.
(3) Activating and soaking nickel: preparing 100mL of activation nickel leaching solution into a 150mL plastic beaker by using deionized water according to the concentration ratio of 25g/L of nickel sulfate, 95mL/L of hydrofluoric acid and 35g/L of boric acid, cleaning the bright substrate material, and placing the substrate material into the activation nickel leaching solution, wherein the reaction time is 5min at room temperature. And taking out the substrate by using tweezers, and then washing the substrate by using deionized water, wherein the surface of the substrate is grayish white.
(4) Alkaline nickel preplating: preparing 100mL of alkaline nickel pre-plating solution by using deionized water according to the concentration ratio of 30g/L of nickel sulfate, 30g/L of sodium hypophosphite and 60g/L of sodium pyrophosphate, and using NH3·H2Adjusting the pH value to 10, putting the base material subjected to the activation nickel leaching treatment into a beaker filled with an alkaline nickel pre-plating solution, putting the beaker into a constant-temperature water bath kettle at 45 ℃, performing alkaline nickel pre-plating treatment for 5min, taking out the base material with tweezers, and then washing the base material with deionized water.
(5) Acid chemical nickel plating: according to the concentration proportion of 26g/L of main salt nickel sulfate, 32g/L of reducing agent sodium hypophosphite, 15mL/L of complexing agent lactic acid, 10g/L of complexing agent citric acid, 15g/L of buffering agent anhydrous sodium acetate and 1g/L of accelerator sodium fluoride, the prepared loading capacity (the ratio of the surface area of a workpiece immersed in the plating solution to the volume of the plating solution) is about 1dm2Acid nickel plating solution of/L, using NH3·H2Blend of oxygen and sulfurThe pH was adjusted to 4.6. The basic material which is subjected to alkaline pre-nickel plating is washed clean by deionized water and then quickly placed into a small beaker filled with acidic nickel plating solution, the mouth of the beaker is wrapped by a preservative film and placed into a constant-temperature water bath kettle at 88 ℃ for reaction for 12 hours, and the acidic plating solution is changed every 1 hour.
And (4) analyzing results: as can be seen from the SEM image of the Ni-P film thickness in FIG. 1, after the treatment of activating nickel immersion, alkaline pre-nickel plating, acid nickel plating and other processes for different time, the thickness of the nickel-phosphorus film on the surface of the aluminum alloy composite material can reach 80-140 μm, the average plating speed is about 11 μm/h, and the film distribution is uniform.
And (4) analyzing results: as can be seen from the SEM of the surface topography of the Ni-P film layer in FIG. 2, the film layer is tightly bonded and dense.
And (4) analyzing results: as can be seen from the XRD diffraction pattern of the surface morphology of the Ni-P film layer in figure 3, a very obvious broadened diffraction peak appears when the diffraction angle 2 theta is about 44-45 degrees, and the position of the amorphous Ni-P diffraction peak is analyzed, which shows that the main component of the surface of the film layer is Ni-P alloy.
And (4) analyzing results: as can be seen from the EDS spectrum of the Ni-P film of fig. 4, the Ni content of the film was about 83.56% and the P content was 16.44% over the selected area.
It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the invention and these are intended to be within the scope of the invention.
Claims (5)
1. A preparation method for plating a Ni-P film on the surface of an aluminum alloy substrate is characterized by comprising the following steps: the method comprises the following steps:
firstly, preprocessing an aluminum alloy base material: the method comprises the steps of sanding with sand paper, ultrasonic cleaning, oil removal and alkaline etching;
step two, performing light-emitting treatment on the aluminum alloy base material by using a solution prepared from nitric acid, hydrofluoric acid and water;
step three, activating and nickel-immersing the aluminum alloy base material by using nickel sulfate, hydrofluoric acid and boric acid solution;
step four, mixingThe aluminum alloy base material is subjected to alkaline nickel preplating treatment by using nickel sulfate, sodium hypophosphite and sodium pyrophosphate, and the solution ratio is as follows: nickel sulfate 25-30 g/L, sodium hypophosphite 25-30 g/L, sodium pyrophosphate 50-60 g/L, NH3·H2Adjusting the pH value to about 10 by O, controlling the reaction temperature to 45 ℃ and controlling the reaction time to 5 min;
step five, performing acid chemical nickel plating treatment on the aluminum alloy base material: 25-30 g/L nickel sulfate, 30-35 g/L sodium hypophosphite, 15-20 mL/L lactic acid, 5-10 g/L citric acid, 15-20 g/L anhydrous sodium acetate, 1g/L sodium fluoride, and NH3·H2Adjusting the pH value to 4.5-4.6 by O, and the loading capacity is about 1dm2and/L, the reaction temperature is 88 ℃, and the plating solution is changed every 1 hour.
2. The method for preparing Ni-P film on the surface of Al alloy substrate according to claim 1, wherein: in the first step, the types of the used sand paper are as follows: 120#, 240#, 600#, 1000#, 1500 #; the solvents for ultrasonic cleaning were: absolute ethyl alcohol, and the cleaning time is 10 min; solution proportioning for oil removal and alkaline etching: 20g/L of sodium carbonate, 30g/L of sodium phosphate, 5g/L of sodium hydroxide, 50 ℃ of reaction temperature and 3-5 min of reaction time.
3. The method for preparing Ni-P film on surface of Al alloy substrate according to claim 1 or 2, wherein: in the second step, the used brightening liquid is as follows: nitric acid, hydrofluoric acid and water in a ratio of 3:1:1, wherein the reaction time is 3-5 s.
4. The method for preparing Ni-P film on surface of Al alloy substrate according to claim 3, wherein: in the third step, the proportion of the activating nickel-leaching solution is as follows: 25-30 g/L of nickel sulfate, 90-100 mL/L of hydrofluoric acid and 30-40 g/L of boric acid, and the reaction time is 5min at room temperature.
5. The method for preparing Ni-P film on surface of Al alloy substrate according to claim 3, wherein: cleaning steps are added among the steps, and in the cleaning steps, deionized water is adopted to clean the aluminum alloy base material, and then the next step is carried out.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010730674.2A CN111893464A (en) | 2020-07-27 | 2020-07-27 | Preparation method for plating Ni-P film on surface of aluminum alloy substrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010730674.2A CN111893464A (en) | 2020-07-27 | 2020-07-27 | Preparation method for plating Ni-P film on surface of aluminum alloy substrate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111893464A true CN111893464A (en) | 2020-11-06 |
Family
ID=73190976
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010730674.2A Pending CN111893464A (en) | 2020-07-27 | 2020-07-27 | Preparation method for plating Ni-P film on surface of aluminum alloy substrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111893464A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113430591A (en) * | 2021-06-29 | 2021-09-24 | 深圳市精一新材料控股(集团)有限公司 | Surface treatment process of aluminum alloy |
| CN115216626A (en) * | 2022-06-10 | 2022-10-21 | 杭州航天电子技术有限公司 | Ultrasonic nickel leaching device and method for aluminum alloy surface treatment |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3666529A (en) * | 1969-04-02 | 1972-05-30 | Atomic Energy Commission | Method of conditioning aluminous surfaces for the reception of electroless nickel plating |
| CN101319316A (en) * | 2008-06-25 | 2008-12-10 | 广东工业大学 | Method for chemical nickel plating on aluminum and aluminum alloy surface |
| CN102747345A (en) * | 2012-07-19 | 2012-10-24 | 哈尔滨工业大学 | Method for chemically plating nickel on surface of copper circuit of PCB (printed circuit board) by dipping and activating nickel |
| CN103014681A (en) * | 2012-12-12 | 2013-04-03 | 西安科技大学 | Preparation method of Ni-P alloy gradient coating |
| CN108034932A (en) * | 2017-12-12 | 2018-05-15 | 云南昆船机械制造有限公司 | A kind of process of 7A19 aluminum alloy material surfaces chemical nickel phosphorus plating |
-
2020
- 2020-07-27 CN CN202010730674.2A patent/CN111893464A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3666529A (en) * | 1969-04-02 | 1972-05-30 | Atomic Energy Commission | Method of conditioning aluminous surfaces for the reception of electroless nickel plating |
| CN101319316A (en) * | 2008-06-25 | 2008-12-10 | 广东工业大学 | Method for chemical nickel plating on aluminum and aluminum alloy surface |
| CN102747345A (en) * | 2012-07-19 | 2012-10-24 | 哈尔滨工业大学 | Method for chemically plating nickel on surface of copper circuit of PCB (printed circuit board) by dipping and activating nickel |
| CN103014681A (en) * | 2012-12-12 | 2013-04-03 | 西安科技大学 | Preparation method of Ni-P alloy gradient coating |
| CN108034932A (en) * | 2017-12-12 | 2018-05-15 | 云南昆船机械制造有限公司 | A kind of process of 7A19 aluminum alloy material surfaces chemical nickel phosphorus plating |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113430591A (en) * | 2021-06-29 | 2021-09-24 | 深圳市精一新材料控股(集团)有限公司 | Surface treatment process of aluminum alloy |
| CN115216626A (en) * | 2022-06-10 | 2022-10-21 | 杭州航天电子技术有限公司 | Ultrasonic nickel leaching device and method for aluminum alloy surface treatment |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101319316B (en) | Method for chemical nickel plating on aluminum and aluminum alloy surface | |
| CN100464007C (en) | Process for preparing neodymium-iron-boron permanent magnetic material surface gradient function coating layer | |
| CN108165165B (en) | Preparation method of neodymium iron boron magnet material surface composite anticorrosive coating | |
| CN111893464A (en) | Preparation method for plating Ni-P film on surface of aluminum alloy substrate | |
| US20150251216A1 (en) | Magnesium Alloy with Dense Surface Texture and Surface Treatment Method Thereof | |
| CN107779713B (en) | A kind of beryllium alumin(i)um alloy and preparation method thereof | |
| CN104005026A (en) | Method for preparing corrosion-resistant super-hydrophobic membrane layer on surface of magnesium alloy | |
| WO2017101711A1 (en) | Film forming treatment agent for composite chemical conversion film for magnesium alloy, and film forming process | |
| CN114574022B (en) | Preparation method of low-surface-energy nano coating on surface of magnesium alloy | |
| CN108034932A (en) | A kind of process of 7A19 aluminum alloy material surfaces chemical nickel phosphorus plating | |
| CN112126929A (en) | Local gold plating process for surface of aluminum material | |
| CN105887056A (en) | Chemical nickel plating method for surface of magnesium alloy | |
| CN101871101A (en) | Preparation method of magnesium alloy surface metal plating layer | |
| CN101619448A (en) | Pretreatment solution used for electroless nickel-phosphorus alloy plating layer on surface of aluminum alloy | |
| JP5937086B2 (en) | Electroless metal deposition using highly alkaline plating bath | |
| CN102817019A (en) | Plating solution for chemical plating of nickel-phosphorus metal layer on surface of magnesium alloy as well as preparation and use method for plating solution | |
| CN111286770B (en) | Composite material with high binding force | |
| CN1304633C (en) | Chemical nickel-plating method on magnesium alloy surface | |
| CN1421547A (en) | Electroplating of Zn-Ni alloy onto surface of Nd-Fe-B permanent magnet | |
| JP7285370B2 (en) | Method for synchronous metallization of metallic and non-metallic layers in PCB aluminum substrate holes | |
| CN111910179A (en) | Method for plating Ni-P film on surface of SiCp/Al composite material | |
| CN114934268B (en) | Magnesium alloy chemical nickel-phosphorus plating solution and plating process thereof | |
| CN111364030A (en) | Pretreatment method for improving flatness of electroless NiP plating layer on aluminum substrate | |
| CN110195244A (en) | A method of for inhibiting printed circuit board electrotinning tin one of the main divisions of the male role in traditional opera long | |
| CN116145138A (en) | Magnesium alloy surface anti-corrosion treatment method and metal anti-corrosion coating |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20201106 |
|
| RJ01 | Rejection of invention patent application after publication |