CN102618855B - Preparation method of Ni-P-Al2O3 nanometer composite coating - Google Patents
Preparation method of Ni-P-Al2O3 nanometer composite coating Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 238000000576 coating method Methods 0.000 title claims abstract description 32
- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 239000011248 coating agent Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910052593 corundum Inorganic materials 0.000 title abstract 3
- 229910001845 yogo sapphire Inorganic materials 0.000 title abstract 3
- 238000000034 method Methods 0.000 claims abstract description 29
- 238000000227 grinding Methods 0.000 claims abstract description 23
- 239000000126 substance Substances 0.000 claims abstract description 22
- 239000002245 particle Substances 0.000 claims abstract description 19
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- 239000007787 solid Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 230000008569 process Effects 0.000 claims abstract description 5
- 238000010533 azeotropic distillation Methods 0.000 claims abstract description 3
- 238000007747 plating Methods 0.000 claims description 29
- 239000000463 material Substances 0.000 claims description 15
- 238000013019 agitation Methods 0.000 claims description 12
- 239000012530 fluid Substances 0.000 claims description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000002114 nanocomposite Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000000919 ceramic Substances 0.000 claims description 8
- 239000000758 substrate Substances 0.000 claims description 7
- 230000004913 activation Effects 0.000 claims description 6
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 claims description 6
- 229910018104 Ni-P Inorganic materials 0.000 claims description 5
- 229910018536 Ni—P Inorganic materials 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 230000002572 peristaltic effect Effects 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- 238000004381 surface treatment Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001704 evaporation Methods 0.000 claims description 4
- 230000008020 evaporation Effects 0.000 claims description 4
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 4
- 238000007669 thermal treatment Methods 0.000 claims description 4
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 4
- MIMUSZHMZBJBPO-UHFFFAOYSA-N 6-methoxy-8-nitroquinoline Chemical compound N1=CC=CC2=CC(OC)=CC([N+]([O-])=O)=C21 MIMUSZHMZBJBPO-UHFFFAOYSA-N 0.000 claims description 3
- 244000137852 Petrea volubilis Species 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 150000002815 nickel Chemical class 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 3
- 239000001384 succinic acid Substances 0.000 claims description 3
- HRXKRNGNAMMEHJ-UHFFFAOYSA-K trisodium citrate Chemical compound [Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O HRXKRNGNAMMEHJ-UHFFFAOYSA-K 0.000 claims description 3
- 229940038773 trisodium citrate Drugs 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 abstract description 6
- 229910001018 Cast iron Inorganic materials 0.000 abstract description 3
- 239000002105 nanoparticle Substances 0.000 abstract description 3
- 230000002829 reductive effect Effects 0.000 abstract description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052759 nickel Inorganic materials 0.000 abstract description 2
- 239000011574 phosphorus Substances 0.000 abstract description 2
- 229910052698 phosphorus Inorganic materials 0.000 abstract description 2
- 230000008859 change Effects 0.000 description 4
- 150000001875 compounds Chemical class 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 238000010183 spectrum analysis Methods 0.000 description 4
- 239000004411 aluminium Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 230000007797 corrosion Effects 0.000 description 3
- 238000007772 electroless plating Methods 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
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- 239000003795 chemical substances by application Substances 0.000 description 2
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- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
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- -1 carbide Chemical class 0.000 description 1
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- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
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- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a Ni-P-Al2O3 nanometer composite coating and a preparation method thereof. According to the invention, a wet alumina ceramic agitated bead mill ultrafine grinding process with high energy density and an azeotropic distillation drying process are combinedly used to prepare dispersed nanoparticle-level pure solid alumina powder with an average particle size of 12 nanometers, and then nanometer alumina particles are added into a chemical coating bath and deposit, together with nickel and phosphorus, on the surface of a cast iron workpiece so as to form the Ni-P-Al2O3 nanometer composite coating. The nanometer alumina particles prepared by the method provided in the invention can improve the hardness and wear resistance of the coating and enhance wear resistance of a mechanical part, thereby improving the service life of the coating; not only preparation cost for the composite coating is reduced, but also the composite coating having the advantages of uniformity, low porosity and excellent wear resistance is obtained.
Description
Technical field
The present invention relates to ni-p electroless plating field, specifically a kind of Ni-P-Al
2o
3nano-composite plate and preparation method thereof.
Background technology
Chemical nickel plating is to use reductive agent that the nickel ion reduce deposition in solution is had on the surface of catalytic activity.But simple alloy layer can not meet various industrial sectors sometimes to many-sided requirements such as coating hardness, wear resistance, solidity to corrosion, self lubricity, electroconductibility, therefore studied in large quantities the compound phase coating of the solid, inert particulate that adulterates both at home and abroad in alloy.Nano material has good performance, so Application of micron has caused widely and paid close attention to the Technology of composite chemical coating technology.People have also prepared the composite deposite of various features in succession, as superhard wear coating, self-lubricating coating, protection against corrosion coating, electroconductive coating, decorative coating etc.The patent of having invented has: the preparation method of self-lubricating chemical composite plating (CN200510025066.7), a kind of middle temperature acidic nanometer chemical composition plating Ni-P-Al
2o
3technical recipe (CN201010500630.7), fiber-optic grating sensor electroless composite plating-ZrO
2method (CN200810061209.3),
oneplant high phosphorus Ni-P-SiC composite deposite and preparation technology (CN200710015538.X) thereof, nickel-base composite coat of a kind of wear resistant friction reducing and preparation method thereof (CN200510061588.2), the method (CN200710067634.9) of preparing nanometer antiwear composite coating at metal base surface, processing method prepared by Ni-P-Ni/SiC composite deposite (CN200810137036.9), the method of enhancing nickel-phosphorus composite deposit by using modified nano silicon dioxide particles (CN201010253728.7), chemical depositing Ni-P-nano titanic oxide photocatalysis composite and solution and coating method thereof (CN200910116004.5).
Oneself a kind of utmost point of being considered to the problems such as current solution high temperature corrosion, hot strength and wearing and tearing of Ni-P has the method for application prospect, is a kind of advanced method of producing composite surface material.Therefore,, through the fast development of nearly decades, Ni-P has become one of most active field of surface engineering technique.
Along with research in recent years, for the insoluble solid particle of Composite Coatings, from oxide compound, carbide, nitride, expand to the pottery grain husk grain of present nearly all type, various metal-powder, toner and graphite, MoS
2, WS, tetrafluoroethylene, diamond etc. all can be used as the particle of plating.But the second-phase insoluble particle that obtains former studies and application all adopts chemical method to prepare, therefore, there is the comparatively shortcoming such as complexity of the high and subsequent treatment process of preparation cost.Low-cost preparation, technique ceramic agitation beads grinding machine extra-fine grinding wet method simple and high-energy-density that can nearly " zero " contamination particle of output is prepared the nano-ceramic particle that can be used for Composite Coatings effectively, and can be used for the composite deposite that preparation interpolation and chemical method are prepared the identical excellent property of nano-ceramic particle.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of Ni-P-Al is provided
2o
3nano-composite plate and preparation method thereof.It is compound second phase particles that the present invention adopts the nano aluminium oxide that nearly " zero " prepared by a kind of ceramic agitation beads grinding machine extra-fine grinding wet method of high-energy-density pollutes, and adopts the nickel-phosphorus composite deposit of the nano aluminium oxide that the method preparation of electroless plating contains extra-fine grinding.
Realizing the technical scheme that the object of the invention adopts comprises:
A kind of Ni-P-Al
2o
3the preparation method of nano-composite plate, comprises the steps:
(1) prepare nano alumina particles
First, the micron order alumina raw material slip that configuration solid masses concentration is 30%, by peristaltic pump, slip is pumped into Laboratary type ball mill pottery mill chamber, peristaltic pump rotating speed is made as 25rpm, zirconium white mill pearl pearl footpath: 0.4~0.6 mm, and the ceramic runner rotating speed of grinding machine is 2500rpm, alumina-ceramic grinding chamber internal pressure: 0.03MPa, grinding temperature: 65 ℃, circular grinding, after 12 hours, obtains alumina in Nano level slip; This alumina in Nano level slip is dry, obtain nano aluminium oxide pressed powder;
(2) surface treatment of body material
By the polishing of substrate material surface process, polishing, rust cleaning, oil removing and acid-wash activation operation;
(3) configuration of chemical plating fluid
With deionized water, be configured to the chemical plating fluid of 300ml, comprise: single nickel salt: 30 g/L, inferior sodium phosphate: 30 g/L, Trisodium Citrate: 9 g/L, succinic acid: 12 g/L, lactic acid: 7 g/L, oxysuccinic acid: 9 g/L, ammonium bifluoride: 1 g/L, and nano aluminium oxide: 0.5~2 g/L;
(4) Ni-P
By the above-mentioned chemical plating fluid configuring, with ammoniacal liquor, regulate pH value in 5.2~5.5, then be warming up to 70 ℃, the good body material of surface treatment is placed in to chemical plating fluid plating 90 minutes, keeping magnetic agitation speed is 200rpm, can obtain composite deposite at substrate material surface;
(5) coating thermal treatment
The electric furnace that the composite deposite of above-mentioned gained is placed in to 350 ℃ is incubated 1 hour, can obtain required Ni-P-Al
2o
3nano-composite plate.
The dry azeotropic distillation drying that adopts of alumina in Nano level slip in described step (1), comprises: evaporation together with after the water that is 4.43% by mass percent mixes with 95.57% ethanol, after treating ethanol evaporation, can obtain nano aluminium oxide pressed powder.
The sand paper order number that in described step (2), substrate material surface is polished used is followed successively by 400 orders, 800 orders, 1000 orders, 1500 orders; Adopt the HCl solution rust cleaning that mass percent is 50%; Adopt NaOH and Na
3pO
4be the mixing solutions oil removing of 1:1 by weight; The HCl solution soaking 30s that employing mass percent is 10% is with activation substrate material surface.
In described step (4), chemical plating fluid also needs to disperse through the ultrasonic dispersion of 0.5 hour and the magnetic agitation of 1 hour before plating, and wherein in magnetic agitation groove, zirconium oxide bead pearl footpath is 0.3~0.5mm, and magnetic agitation rotating speed is 200rpm.
Another object of the present invention is to provide a kind of Ni-P-Al being prepared from by aforesaid method
2o
3nano-composite plate.
Compared with prior art, the present invention has the following advantages and beneficial effect:
(1) to adopt the nano aluminium oxide that nearly " zero " prepared by a kind of ceramic agitation beads grinding machine extra-fine grinding wet method of high-energy-density pollutes be compound second phase particles to the inventive method, and the Nano-Particles Composite Coating that obtains preparing to chemical method is at the hardness coating similar with wear resisting property, this measure can reduce the preparation cost for composite deposite nano particle.
(2) Ni-P-Al that prepared by the inventive method
2o
3nano-composite plate is all better than the common coating of Ni-P on hardness, wear resisting property.
(3) the inventive method adopts electroless plating method, the method does not rely on impressed current, only depend on the reductive agent in plating solution to carry out redox reaction, under the self-catalysis of metallic surface, make metal ion constantly be deposited on metallic surface, therefore, apparatus and process is simple, does not need power supply and electrode system during operation, only need be by workpiece suspension in plating solution; Compare with electrolytic coating, chemical plating is not subject to the restriction of complex part complex configuration, even thickness, and porosity is lower, strong with basal body binding force.
(4) the present invention adopts azeotropic drying method dry, compares can obtain dispersed nano-powder preferably with forced air drying method.
Accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention 1 nano alumina particles particle diameter and specific surface are with milling time change curve;
Fig. 2 is the embodiment of the present invention 1 nano alumina particles scanning electron microscope (SEM) photograph;
Fig. 3 is the embodiment of the present invention 1 composite deposite surface topography map;
Fig. 4 is the energy spectrum analysis figure of the embodiment of the present invention 1 composite deposite.
Embodiment
Below in conjunction with specific embodiment, the present invention is more specifically described in detail, but embodiments of the present invention are not limited to this, for not dated especially processing parameter, can carry out with reference to routine techniques.
The alumina raw material slip that configuration solid content is 30%, by peristaltic pump, slip is pumped into WLB-0.3G Laboratary type ball mill pottery mill chamber, when feeding coal is 1.5l/min, grinding zirconium oxide bead footpath is 0.4-0.6 mm, the ceramic runner rotating speed of grinding machine is 2500rpm, circular grinding 12 hours, obtaining median size is nearly " zero " pollution alumina in Nano level slip of 12 nanometers, as shown in Figure 1.By the method in above-mentioned second step, carry out azeotropic drying, obtain the nano alumina particles of good dispersion, surface clean, as shown in Figure 2.
Cast iron (10*10*10mm) material is through these five operations of polishing-polishing-rust cleaning-oil removing-acid-wash activation.The sand paper order number of wherein polishing used is followed successively by 400 orders, 800 orders, 1000 orders, 1500 orders.Adopt 50% HCl solution rust cleaning, NaOH and Na
3pO
4mixing solutions (wt1:1) oil removing, 10% HCl solution soaking 30s with activation matrix surface.
By deionized water configuration 300ml plating solution for following various material conditions.
Single nickel salt: 30 g/L inferior sodium phosphate: 30 g/L
Trisodium Citrate: 9 g/L succinic acid: 12 g/L
Lactic acid: 7 g/L oxysuccinic acid: 9 g/L
Ammonium bifluoride: nano aluminium oxide prepared by 1 g/L extra-fine grinding: 0.5 g/L
With ammoniacal liquor, regulate pH value in 5.2-5.5, the chemical composite plating bath that contains nano aluminium oxide prepared by extra-fine grinding disperses (steel basin includes the zirconium oxide bead that pearl footpath is 0.3-0.5mm) through the ultrasonic dispersion of 0.5 hour and the high speed magnetic stirring of 1 hour before plating, and stirring velocity is 800rpm.
Treat that bath temperature rises to 70 ℃ and insulation, keeping magnetic agitation speed is that 200rpm is to guarantee the good dispersion suspension state of nano alumina particles, the good body material of surface treatment is placed in to scattered chemical plating fluid plating 90 minutes, take out plating piece, dry to be placed in electric furnace and be incubated 1 hour at 350 ℃, acquisition is deposited on the composite deposite of Cast Iron Surface, as shown in Figure 3.The coating aluminium content obtaining through energy spectrum analysis is 3.77%, and as shown in Figure 4, the heat treated vickers microhardness of coating is 904HV.
embodiment 2:
Press the same step of embodiment 1, but the addition of the nano aluminium oxide that in change plating solution prepared by extra-fine grinding is 1g/L.The coating aluminium content obtaining through energy spectrum analysis is 3.94%, and the vickers microhardness after coating thermal treatment is 930HV.
Press the same step of embodiment 1, but the addition of the nano aluminium oxide that in change plating solution prepared by extra-fine grinding is 2g/L.The coating aluminium content obtaining through energy spectrum analysis is 3.94%, and the vickers microhardness after coating thermal treatment is 1016HV.
Above-described embodiment is preferably embodiment of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other any do not deviate from change, the modification done under spirit of the present invention and principle, substitutes, combination, simplify; all should be equivalent substitute mode, within being included in protection scope of the present invention.
Claims (3)
1. a Ni-P-Al
2o
3the preparation method of nano-composite plate, is characterized in that, comprises the steps: that (1) prepare nano alumina particles
First, the micron order alumina raw material slip that configuration solid masses concentration is 30%, by peristaltic pump, slip is pumped into Laboratary type ball mill pottery mill chamber, peristaltic pump rotating speed is made as 25rpm, zirconium white mill pearl pearl footpath: 0.4~0.6 mm, and the ceramic runner rotating speed of grinding machine is 2500rpm, alumina-ceramic grinding chamber internal pressure: 0.03MPa, grinding temperature: 65 ℃, circular grinding, after 12 hours, obtains alumina in Nano level slip; This alumina in Nano level slip is dry, obtain nano aluminium oxide pressed powder; Describedly specifically adopt azeotropic distillation drying by alumina in Nano level slip is dry: evaporation together with after the water that is 4.43% by mass percent mixes with 95.57% ethanol, after treating ethanol evaporation, can obtain nano aluminium oxide pressed powder;
(2) surface treatment of body material
By the polishing of substrate material surface process, polishing, rust cleaning, oil removing and acid-wash activation operation;
(3) configuration of chemical plating fluid
With deionized water, be configured to the chemical plating fluid of 300ml, comprise: single nickel salt: 30 g/L, inferior sodium phosphate: 30 g/L, Trisodium Citrate: 9 g/L, succinic acid: 12 g/L, lactic acid: 7 g/L, oxysuccinic acid: 9 g/L, ammonium bifluoride: 1 g/L, and nano aluminium oxide: 0.5~2 g/L;
(4) Ni-P
By the above-mentioned chemical plating fluid configuring, with ammoniacal liquor, regulate pH value in 5.2~5.5, then be warming up to 70 ℃, the good body material of surface treatment is placed in to chemical plating fluid plating 90 minutes, keeping magnetic agitation speed is 200rpm, can obtain composite deposite;
(5) coating thermal treatment
The electric furnace that the composite deposite of above-mentioned gained is placed in to 350 ℃ is incubated 1 hour, can obtain required Ni-P-Al
2o
3nano-composite plate.
2. preparation method according to claim 1, is characterized in that, the sand paper order number that in step (2), substrate material surface is polished used is followed successively by 400 orders, 800 orders, 1000 orders, 1500 orders; Adopt the HCl solution rust cleaning that mass percent is 50%; Adopt NaOH and Na
3pO
4be the mixing solutions oil removing of 1:1 by weight; The HCl solution soaking 30s that employing mass percent is 10% is with activation substrate material surface.
3. preparation method according to claim 1, it is characterized in that, in step (4), chemical plating fluid also needs to disperse through the ultrasonic dispersion of 0.5 hour and the magnetic agitation of 1 hour before plating, wherein in magnetic agitation groove, zirconium oxide bead pearl footpath is 0.3~0.5mm, and magnetic agitation rotating speed is 200rpm.
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CN116043200A (en) * | 2022-12-28 | 2023-05-02 | 国家石油天然气管网集团有限公司 | Preparation method of nickel-phosphorus-based hydrogen-resistant composite coating |
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