CN112663031A - Ultra-thick high-phosphorus chemical nickel plating and stabilizing treatment process for aluminum-based silicon carbide composite material - Google Patents
Ultra-thick high-phosphorus chemical nickel plating and stabilizing treatment process for aluminum-based silicon carbide composite material Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 233
- 238000007747 plating Methods 0.000 title claims abstract description 145
- 239000000126 substance Substances 0.000 title claims abstract description 125
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 116
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 61
- 239000011574 phosphorus Substances 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 54
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 44
- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 230000008569 process Effects 0.000 title claims abstract description 43
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 43
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 41
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 41
- 230000000087 stabilizing effect Effects 0.000 title claims description 23
- 238000007598 dipping method Methods 0.000 claims abstract description 51
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 48
- 239000011701 zinc Substances 0.000 claims abstract description 48
- 238000005260 corrosion Methods 0.000 claims abstract description 19
- 230000007797 corrosion Effects 0.000 claims abstract description 18
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims description 74
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 31
- 238000004140 cleaning Methods 0.000 claims description 20
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 12
- 230000008021 deposition Effects 0.000 claims description 12
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 claims description 10
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 9
- 239000011248 coating agent Substances 0.000 claims description 9
- 238000000576 coating method Methods 0.000 claims description 9
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 9
- 239000000395 magnesium oxide Substances 0.000 claims description 9
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 7
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 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 6
- 229910021205 NaH2PO2 Inorganic materials 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 6
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 claims description 5
- 238000005485 electric heating Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 4
- 239000003921 oil Substances 0.000 claims description 4
- FJMNNXLGOUYVHO-UHFFFAOYSA-N aluminum zinc Chemical compound [Al].[Zn] FJMNNXLGOUYVHO-UHFFFAOYSA-N 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 238000005238 degreasing Methods 0.000 claims description 3
- 238000005530 etching Methods 0.000 claims description 3
- 238000009472 formulation Methods 0.000 claims description 3
- 230000006698 induction Effects 0.000 claims description 3
- 238000011068 loading method Methods 0.000 claims description 3
- QPJSUIGXIBEQAC-UHFFFAOYSA-N n-(2,4-dichloro-5-propan-2-yloxyphenyl)acetamide Chemical compound CC(C)OC1=CC(NC(C)=O)=C(Cl)C=C1Cl QPJSUIGXIBEQAC-UHFFFAOYSA-N 0.000 claims description 3
- 229910000008 nickel(II) carbonate Inorganic materials 0.000 claims description 3
- ZULUUIKRFGGGTL-UHFFFAOYSA-L nickel(ii) carbonate Chemical compound [Ni+2].[O-]C([O-])=O ZULUUIKRFGGGTL-UHFFFAOYSA-L 0.000 claims description 3
- 235000011837 pasties Nutrition 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 239000000523 sample Substances 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000012085 test solution Substances 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 7
- 238000006555 catalytic reaction Methods 0.000 abstract description 6
- 238000006243 chemical reaction Methods 0.000 abstract description 5
- 150000003839 salts Chemical class 0.000 abstract description 5
- 230000008719 thickening Effects 0.000 abstract description 5
- 238000004886 process control Methods 0.000 abstract description 4
- 239000003638 chemical reducing agent Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 229910001453 nickel ion Inorganic materials 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 150000002815 nickel Chemical class 0.000 description 3
- 230000003287 optical effect Effects 0.000 description 3
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- YZCKVEUIGOORGS-UHFFFAOYSA-N Hydrogen atom Chemical group [H] YZCKVEUIGOORGS-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 229910001096 P alloy Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
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- 230000002269 spontaneous effect Effects 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
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Abstract
The process is characterized in that aiming at the high-strength and low-weight aluminum-based silicon carbide composite material, through adopting proper pretreatment corrosion and chemical nickel pre-plating process, oxide on the surface of the material can be removed, corrosion can not be generated, the binding force of a plating layer is improved, through the processes of primary zinc dipping, gloss treatment, secondary zinc dipping, chemical nickel pre-plating, high-phosphorus chemical nickel plating and the like, through the process control methods of temperature step heating, control of main salt concentration and the like, the normal running and continuous thickening of catalytic reaction are maintained, the thickness of the chemical nickel plating layer is improved, the surface of the chemical nickel plating layer is uniform, flat and smooth, a unique vacuum stable treatment method is adopted, the stress of the plating layer is eliminated, and the problem that the chemical nickel plating binding force of the aluminum-based silicon carbide composite material is poor is solved, the chemical nickel plating reaction is stopped, and the chemical nickel plating layer can not be thickened continuously.
Description
Technical Field
The invention belongs to the technical field of novel composite material chemical nickel plating processes, and particularly relates to an ultra-thick high-phosphorus chemical nickel plating and stabilizing treatment process for an aluminum-based silicon carbide composite material.
Background
The aluminum-based silicon carbide composite material has higher specific strength, specific elastic modulus, low weight and excellent comprehensive performance, and is widely applied to the advanced fields of space reflectors, microwave integrated circuits, power modules, high-speed rails and the like. The aluminum-based silicon carbide composite material is a multiphase composite material which takes hard aluminum alloy as a base, takes silicon carbide particles (carborundum) as a reinforcement in a certain form, proportion and distribution state and has an obvious interface and has comprehensive superior performance which is not possessed by single metal. Because the silicon carbide particles are semiconductor materials and have excellent chemical corrosion resistance and oxidation resistance, the aluminum base is preferentially corroded when the chemical treatment is carried out, and the silicon carbide particles do not participate in chemical reaction and can be precipitated and adhered to the surface of a part to form uneven surface corrosion and black and gray surface, so that the surface quality of the chemical nickel plating layer is seriously influenced. Therefore, the pretreatment technology of the chemical nickel plating of the aluminum-based silicon carbide composite material is a key technology for ensuring the binding force of the plating layer and the surface quality of the matrix. Secondly, the thickness of the commonly used chemical nickel plating layer is generally (5-8) mu m; the thickness of the chemical nickel plating layer of the impeller on the aircraft engine is generally (25-75) mu m; the thickness of the chemical nickel plating layer of the radiator and the oil nozzle in the automobile industry is generally (10-25) mu m, and the thickness of the chemical nickel plating layer required by the reflector is (100-150) mu m, which is 30 times of the thickness of the common chemical nickel plating layer. The analysis on the chemical nickel plating deposition mechanism is to gradually deposit the nickel-phosphorus alloy on the metal surface through a catalytic reaction, so whether the catalytic reaction can be continuously and stably carried out is a key factor for continuously thickening the thickness of a chemical nickel plating layer and is one of the technical difficulties which must be solved by the invention.
Disclosure of Invention
The technical problems solved by the invention are as follows: the invention provides an ultra-thick high-phosphorus chemical nickel plating and stabilizing treatment process of an aluminum-based silicon carbide composite material, which aims at the aluminum-based silicon carbide composite material with high strength and low weight, and can remove oxides on the surface of the material without over-corrosion by adopting a proper pretreatment corrosion and pre-plating chemical nickel process, thereby improving the binding force of a plating layer; the normal operation of catalytic reaction is maintained and the thickness is continuously increased by adopting the processes of primary zinc dipping, gloss treatment, secondary zinc dipping, pre-plating of chemical nickel, high-phosphorus chemical nickel plating and the like and by adopting process control methods such as temperature step heating, control of main salt concentration and the like, so that the thickness of the chemical nickel plating layer is increased, and the surface of the chemical nickel plating layer is uniform, flat and smooth; and a unique vacuum stabilization treatment method is adopted to eliminate coating stress, and the problems that the chemical nickel plating layer of the aluminum-based silicon carbide composite material has poor bonding force, the chemical nickel plating reaction is stopped, and the chemical nickel plating layer cannot be thickened continuously are solved.
The technical scheme adopted by the invention is as follows: the ultra-thick high-phosphorus chemical nickel plating and stabilizing treatment process of the aluminum-based silicon carbide composite material comprises the following steps of:
step 1): chemical oil removal: firstly, mixing magnesium oxide powder with a proper amount of water into paste, detecting the aluminum-based silicon carbide composite material before plating, then wiping the surface to be plated of the aluminum-based silicon carbide composite material part with the paste magnesium oxide powder, and then flushing the aluminum-based silicon carbide composite material part with flowing water until the water film on the surface of the part is uniform for 30s and does not break;
step 2): acid corrosion: placing the aluminum-based silicon carbide composite material part subjected to chemical degreasing into an acid corrosion solution, wherein the solution process parameters are as follows: temperature: 75-85 ℃, time: cleaning with running water after acid corrosion for 1-3 min;
step 3): zinc dipping treatment for the first time: putting the part into a zinc dipping solution, slightly shaking, and cleaning the part with running water, wherein the surface of the part is slightly dark gray after the first zinc dipping; zinc dipping solution parameters: temperature: 15-30 ℃, first zinc dipping time: 60-120 s;
step 4): and (3) gloss treatment: putting the parts subjected to the first zinc dipping treatment into a gloss treatment solution until a zinc dipping layer is completely dissolved to form the natural color of a matrix, and cleaning the parts by running water; the gloss treatment process parameters are as follows: temperature: 10-40 ℃, time: 5-10 s;
step 5): and (3) zinc dipping treatment for the second time: putting the part subjected to the gloss treatment into a zinc dipping solution for secondary zinc dipping treatment, wherein the surface of the part subjected to the secondary zinc dipping treatment is beige, and cleaning the part by running water; wherein, the temperature: 15-30 ℃, and the second zinc dipping time: 30-60 s;
step 6): pre-plating chemical nickel: putting the cleaned parts into a pre-plating chemical nickel bath solution, wherein the time is as follows: 8-12 min, bath solution temperature: 32-38 ℃, pH value: 9.0-9.5, and cleaning with running water;
step 7): high-phosphorus chemical nickel plating: putting the part pre-plated with the chemical nickel into a high-phosphorus chemical nickel plating solution for chemical nickel plating treatment, and cleaning with running water; wherein, the technological parameters of the high-phosphorus chemical nickel plating are as follows: initial temperature: 80-84 ℃, time: 3-4 h, temperature: 85-88 ℃, time: coating to a specified thickness, pH value: 4.6-5.0, deposition rate: 8-12 μm/h;
step 8): and (3) stabilizing treatment: putting the part subjected to high-phosphorus chemical nickel plating into a vacuum drying oven for stabilizing; and (3) stabilizing treatment process parameters: temperature: and (2) at 180-200 ℃, time: 3-4 h, vacuum degree: 100 to 200Pa-1；
Step 9): and (4) checking: and (5) checking whether the appearance, the thickness, the binding force and the phosphorus content of the plating layer of the part are in accordance with the requirements.
In the step 1), a clean soft brush is used for dipping pasty magnesium oxide powder to wipe the surface to be plated of the aluminum-based silicon carbide composite material part for 2-3 times.
In the step 2), the formula of the acid etching solution is as follows: sulfuric acid H2SO4：ρ＝1.84g/cm3，130～150ml/L。
In the step 3) and the step 5), the formulation of the zinc dipping solution is as follows: aluminum zinc deposition agent W-2000: 500-550 ml/L; pure water class B H2O: and (4) the balance.
In the step 4), the formula of the gloss treatment solution is as follows: 40% nitric acid HNO3：ρ＝1.42g/cm3(ii) a Hydrofluoric acid (HF): rho is 1.12g/cm3，20ml/L。
In the step 6), the formula of the pre-plating chemical nickel solution is as follows:ni ion Ni2+Adding in the form of basic nickel carbonate: 5.6-6.4 g/L; sodium hypophosphite NaH2PO2·3H2O：21～27g/L。
In the step 7), the formula of the high-phosphorus chemical nickel plating solution is as follows: ni ion Ni2+Adding in the form of nickel sulfate: 5.0 to 6.2g/L, sodium hypophosphite NaH2PO2·3H2O: 26-33 g/L; the pH value of the high-phosphorus chemical nickel plating solution is tested by adopting a calibrated acidimeter, the test solution is measured after being cooled to room temperature, nickel sulfate is analyzed and supplemented at any time in the plating process according to the loading amount, and the plating solution is supplemented regularly to keep the pH value relatively stable; circularly filtering the high-phosphorus chemical nickel plating solution by using a chemical nickel plating filter with the filtering precision not lower than 5 mu m, wherein the circulating filtering frequency is 7-10 times/h, and the cleaning of the bath solution is ensured; the heating mode of the high-phosphorus chemical nickel plating solution adopts a stainless steel electric heating tube coated by polytetrafluoroethylene, and is provided with a Pt100 temperature control induction probe, the temperature control precision is +/-0.5 ℃, and the heating reliability and the temperature uniformity are ensured.
Compared with the prior art, the invention has the advantages that:
the scheme aims at the aluminum-based silicon carbide composite material with high strength and low weight, and by adopting the proper pretreatment corrosion and the chemical nickel preplating process, the oxide on the surface of the material can be removed, over corrosion can not be generated, and the binding force of a coating is improved; the normal operation of catalytic reaction is maintained and the thickness is continuously increased by adopting the processes of primary zinc dipping, gloss treatment, secondary zinc dipping, pre-plating of chemical nickel, high-phosphorus chemical nickel plating and the like and by adopting process control methods such as temperature step heating, control of main salt concentration and the like, so that the thickness of a chemical nickel plating layer is increased, the thickness of the chemical nickel plating layer can reach 0.15mm, the phosphorus content reaches 13%, the surface of the chemical nickel plating layer is uniform, flat and smooth, and the bonding force is good; and a unique vacuum stabilization treatment method is adopted to eliminate the coating stress, thereby solving the technical problems that the chemical nickel plating layer of the aluminum-based silicon carbide composite material has poor bonding force, the chemical nickel plating reaction is stopped, and the chemical nickel plating layer can not be thickened continuously; the composite material can be applied to aerospace optical lenses, bearing journals and undercarriage parts; the automobile radiator, the chemical turbine impeller and other industries have strong practicability and popularization.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a diagram of a reflector of example 2 of the present invention after being treated with ultra-thick high phosphorous electroless nickel.
Detailed Description
The following examples of the invention are described in further detail:
example 1:
the ultra-thick high-phosphorus chemical nickel plating and stabilizing treatment process of the aluminum-based silicon carbide composite material, as shown in figure 1, comprises the following steps:
step 1): chemical oil removal: firstly, the magnesium oxide powder is mixed into paste with a proper amount of water, the aluminum-based silicon carbide composite material is detected before plating, then the paste magnesium oxide powder is used for wiping the surface to be plated of the aluminum-based silicon carbide composite material part, and then the aluminum-based silicon carbide composite material part is washed by flowing water until the water film on the surface of the part is uniform for 30s and is not broken. Wherein, a clean soft brush is used for dipping pasty magnesium oxide powder to wipe the surface to be plated of the aluminum-based silicon carbide composite material part for 2-3 times.
Step 2): acid corrosion: and (3) placing the aluminum-based silicon carbide composite material part subjected to chemical degreasing into an acid corrosion solution. The formula of the acid etching solution is as follows: sulfuric acid H2SO4：ρ＝1.84g/cm3130-150 ml/L. Solution process parameters: temperature: 75-85 ℃, time: and (5) cleaning with running water after acid corrosion for 1-3 min.
Step 3): zinc dipping treatment for the first time: putting the part into a zinc dipping solution, slightly shaking, and cleaning the part with running water, wherein the surface of the part is slightly dark gray after the first zinc dipping; zinc dipping solution parameters: temperature: 15-30 ℃, first zinc dipping time: 60-120 s;
step 4): and (3) gloss treatment: and (3) putting the part subjected to the first zinc dipping treatment into a gloss treatment solution until the zinc dipping layer is completely dissolved to form the natural color of the matrix, and cleaning the matrix with running water. The formula of the gloss treatment solution is as follows: 40% nitric acid HNO3：ρ＝1.42g/cm3(ii) a Hydrofluoric acid (HF): rho is 1.12g/cm320 ml/L. The gloss treatment process parameters are as follows:temperature: 10-40 ℃, time: 5 to 10s
Step 5): and (3) zinc dipping treatment for the second time: putting the part subjected to the gloss treatment into a zinc dipping solution for secondary zinc dipping treatment, wherein the surface of the part subjected to the secondary zinc dipping treatment is beige, and cleaning the part by running water; wherein, the temperature: 15-30 ℃, and the second zinc dipping time: 30-60 s;
in the step 3) and the step 5), the formulation of the zinc dipping solution is as follows: aluminum zinc deposition agent W-2000: 500-550 ml/L; pure water class B H2O: and (4) the balance.
Step 6): pre-plating chemical nickel: putting the cleaned parts into a pre-plating chemical nickel bath solution, wherein the time is as follows: 8-12 min, bath solution temperature: 32-38 ℃, pH value: 9.0-9.5, and washing with running water. The formula of the pre-plating chemical nickel solution comprises the following steps: ni ion Ni2+Adding in the form of basic nickel carbonate: 5.6-6.4 g/L; sodium hypophosphite NaH2PO2·3H2O：21～27g/L。
Step 7): high-phosphorus chemical nickel plating: and putting the part pre-plated with the chemical nickel into a high-phosphorus chemical nickel plating solution for chemical nickel plating treatment, and cleaning with running water. Wherein, the technological parameters of the high-phosphorus chemical nickel plating are as follows: initial temperature: 80-84 ℃, time: 3-4 h, temperature: 85-88 ℃, time: coating to a specified thickness, pH value: 4.6-5.0, deposition rate: 8 to 12 μm/h. The formula of the high-phosphorus chemical nickel plating solution comprises the following components: ni ion Ni2+Adding in the form of nickel sulfate: 5.0 to 6.2g/L, sodium hypophosphite NaH2PO2·3H2O：26～33g/L。
The control technology of the ultra-thick high-phosphorus chemical nickel plating process comprises the following steps:
a) control of high phosphorus chemical nickel plating solution composition
The nickel sulfate is the main salt in the chemical nickel plating solution and the source of nickel ions in the plating layer, and the stability of the concentration of the nickel ions is the key point for ensuring the continuous thickening of the plating layer in the super-thick chemical nickel plating process, and the nickel sulfate is analyzed and supplemented at any time in the plating process according to the loading amount. The nickel salt concentration supplement of the high-phosphorus chemical nickel plating solution is shown in table 1.
TABLE 1 chemical nickel plating solution nickel salt concentration supplement table
b) Control of reducing agent in high-phosphorus chemical nickel plating solution
The reducing agent is used for providing active nascent hydrogen atoms through catalytic dehydrogenation and reducing nickel ions into metallic nickel. The influence of the content of the reducing agent on the deposition speed is large, the deposition speed is accelerated along with the increase of the concentration of the reducing agent, but the reducing agent cannot be too high, otherwise, the plating solution is easy to self-decompose, the stability of the plating solution is damaged, and meanwhile, the deposition speed also reaches a limit value.
c) Control of pH value of high-phosphorus chemical nickel plating bath solution
The pH value of the high-phosphorus chemical nickel plating bath solution is low, the appearance color of the plating layer is dark, and the ductility and the binding force of the plating layer are reduced. The pH value is higher, the phosphorus content in the plating layer is reduced, and even the solution failure caused by the spontaneous decomposition of the plating solution can be caused. Therefore, the pH value of the high-phosphorus chemical nickel plating bath solution is tested by adopting a calibrated acidimeter, the test solution needs to be cooled to room temperature for measurement, the pH value can be kept relatively stable by regularly supplementing the plating solution, and the pH value is detected at least once every shift.
d) Control of bath solution temperature
The working temperature range of the high-phosphorus chemical nickel plating solution is (80-88) DEG C, and because of the ultra-thick chemical nickel plating, the initial temperature is too high, the reduction reaction is rapid and violent, the gas is strongly separated out, and the gas flow mark defect is easily generated on the surface of the part; secondly, the deposition of nickel ions is accelerated, microscopic roughness and pinholes are generated on the surface, and in the subsequent thickening process, the defects of bulges, pits and the like can occur. Therefore, the initial temperature needs to be strictly controlled, the chemical nickel plating layer on the bottom layer is ensured to be uniform and compact, and a good foundation is laid for the subsequent continuous thickening.
e) Control of bath impurities
The nitrate pollution of the high-phosphorus chemical nickel plating solution can cause the slow deposition speed, and the phosphorus content in the plating layer is lower than the normal value. Such contamination often occurs after the nitric acid washes the tank without rinsing it clean with sufficient clean water. Suspended impurities and solid nickel salt particles in the high-phosphorus chemical nickel plating solution can cause the surface of a plating layer to be rough and even cause the service life of bath solution to be reduced. Therefore, the plating solution is circularly filtered by using a chemical nickel plating filter with the filtering precision not lower than 5 mu m and a non-metal filter pump, and the circulating filtering frequency is (7-10) times/h, so that the cleaning of the bath solution is ensured.
f) Electrical heating and temperature control device requirements
The heating mode of the high-phosphorus chemical nickel plating solution needs to adopt a stainless steel electric heating tube coated by polytetrafluoroethylene, and is provided with a Pt100 temperature control induction probe, the temperature control precision is +/-0.5 ℃, and the heating reliability and the temperature uniformity are ensured. After each shift, the electric heating rod needs to be taken out, and the nickel layer deposited on the surface of the heating rod needs to be cleaned.
Step 8): and (3) stabilizing treatment: putting the part subjected to high-phosphorus chemical nickel plating into a vacuum drying oven for stabilizing; and (3) stabilizing treatment process parameters: temperature: and (2) at 180-200 ℃, time: 3-4 h, vacuum degree: 100 to 200Pa-1。
Step 9): and (4) checking: and (5) checking whether the appearance, the thickness, the binding force and the phosphorus content of the plating layer of the part are in accordance with the requirements. The specific test method is shown in Table 2.
TABLE 2 quality inspection requirements for ultra-thick high-phosphorus electroless nickel plating
Example 2:
for a certain optical reflector part, the material is aluminum-based silicon carbide, the mark is SiC45/Al YB I grade, and the material standard is as follows: Q/HITCL001-2010 requires high-phosphorus chemical nickel plating, the thickness of a plating layer is 0.12-0.15 mm, the phosphorus content is 10.5-13%, the outer surface of the reflector requires the plating layer to be flat, the defects of air holes, looseness, particles, scratches, flow marks and the like are not allowed, and the bonding force of the plating layer is good.
After the treatment by the process flow and the process method, the appearance, the coating thickness, the binding force and the phosphorus content of the chemical nickel-plating layer of the reflector have four technical indexes, and according to the standard of HB/Z5071-2004 chemical nickel-plating process and quality inspection, the appearance of the coating is semi-glossy silvery white, and the coating does not drop off, peel off and bubble; the thickness of the plating layer reaches (120-140) mu m; the phosphorus content in the plating layer is 13 percent, and the qualification rate reaches 100 percent. And then polishing is carried out to achieve the effect of a metal mirror surface and meet the use requirements of users, as shown in figure 2. The used surface treatment method, the stabilizing treatment process and the implementation result have industrial advancement and uniqueness.
Aiming at the aluminum-based silicon carbide composite material with high strength and low weight, the invention adopts the proper pretreatment corrosion and the chemical nickel preplating process, thereby not only removing the oxide on the surface of the material, but also not generating over corrosion, and improving the binding force of a plating layer; the normal operation of catalytic reaction is maintained and the thickness is continuously increased by adopting the processes of primary zinc dipping, gloss treatment, secondary zinc dipping, pre-plating of chemical nickel, high-phosphorus chemical nickel plating and the like and by adopting process control methods such as temperature step heating, control of main salt concentration and the like, so that the thickness of a chemical nickel plating layer is increased, the thickness of the chemical nickel plating layer can reach 0.15mm, the phosphorus content reaches 13%, the surface of the chemical nickel plating layer is uniform, flat and smooth, and the bonding force is good; and a unique vacuum stabilization treatment method is adopted to eliminate the stress of the plating layer; the technical problems that the chemical nickel plating layer of the aluminum-based silicon carbide composite material is poor in binding force, the chemical nickel plating reaction is stopped, and the chemical nickel plating layer cannot be thickened continuously are solved; the composite material can be applied to the industries of aerospace optical lenses, bearing journals, undercarriage parts, automobile radiators, chemical turbine impellers and the like, and has strong practicability and popularization.
The above-mentioned embodiments are merely preferred embodiments of the present invention, which are not intended to limit the scope of the present invention, and therefore, all equivalent changes made by the contents of the claims of the present invention should be included in the claims of the present invention.
Claims (7)
1. The ultra-thick high-phosphorus chemical nickel plating and stabilizing treatment process of the aluminum-based silicon carbide composite material is characterized by comprising the following steps of: the method comprises the following steps:
step 1): chemical oil removal: firstly, mixing magnesium oxide powder with a proper amount of water into paste, detecting the aluminum-based silicon carbide composite material before plating, then wiping the surface to be plated of the aluminum-based silicon carbide composite material part with the paste magnesium oxide powder, and then flushing the aluminum-based silicon carbide composite material part with flowing water until the water film on the surface of the part is uniform for 30s and does not break;
step 2): acid corrosion: placing the aluminum-based silicon carbide composite material part subjected to chemical degreasing into an acid corrosion solution, wherein the solution process parameters are as follows: temperature: 75-85 ℃, time: cleaning with running water after acid corrosion for 1-3 min;
step 3): zinc dipping treatment for the first time: putting the part into a zinc dipping solution, slightly shaking, and cleaning the part with running water, wherein the surface of the part is slightly dark gray after the first zinc dipping; zinc dipping solution parameters: temperature: 15-30 ℃, first zinc dipping time: 60-120 s;
step 4): and (3) gloss treatment: putting the parts subjected to the first zinc dipping treatment into a gloss treatment solution until a zinc dipping layer is completely dissolved to form the natural color of a matrix, and cleaning the parts by running water; the gloss treatment process parameters are as follows: temperature: 10-40 ℃, time: 5-10 s;
step 5): and (3) zinc dipping treatment for the second time: putting the part subjected to the gloss treatment into a zinc dipping solution for secondary zinc dipping treatment, wherein the surface of the part subjected to the secondary zinc dipping treatment is beige, and cleaning the part by running water; zinc dipping solution parameters: temperature: 15-30 ℃, and the second zinc dipping time: 30-60 s;
step 6): pre-plating chemical nickel: putting the cleaned parts into a pre-plating chemical nickel bath solution, wherein the time is as follows: 8-12 min, bath solution temperature: 32-38 ℃, pH value: 9.0-9.5, and cleaning with running water;
step 7): high-phosphorus chemical nickel plating: putting the part pre-plated with the chemical nickel into a high-phosphorus chemical nickel plating solution for chemical nickel plating treatment, and cleaning with running water; wherein, the technological parameters of the high-phosphorus chemical nickel plating are as follows: initial temperature: 80-84 ℃, time: 3-4 h, temperature: 85-88 ℃, time: coating to a specified thickness, pH value: 4.6-5.0, deposition rate: 8-12 μm/h;
step 8): and (3) stabilizing treatment: putting the part subjected to high-phosphorus chemical nickel plating into a vacuum drying oven for stabilizing; and (3) stabilizing treatment process parameters: temperature: and (2) at 180-200 ℃, time: 3-4 h, vacuum degree: 100 to 200Pa-1；
Step 9): and (4) checking: and (5) checking whether the appearance, the thickness, the binding force and the phosphorus content of the plating layer of the part are in accordance with the requirements.
2. The ultra-thick high-phosphorus chemical nickel plating and stabilizing treatment process for the aluminum-based silicon carbide composite material according to claim 1, is characterized in that: in the step 1), a clean soft brush is used for dipping pasty magnesium oxide powder to wipe the surface to be plated of the aluminum-based silicon carbide composite material part for 2-3 times.
3. The ultra-thick high-phosphorus chemical nickel plating and stabilizing treatment process for the aluminum-based silicon carbide composite material according to claim 1, is characterized in that: in the step 2), the formula of the acid etching solution is as follows: sulfuric acid H2SO4：ρ＝1.84g/cm3，130～150ml/L。
4. The ultra-thick high-phosphorus chemical nickel plating and stabilizing treatment process for the aluminum-based silicon carbide composite material according to claim 1, is characterized in that: in the step 3) and the step 5), the formulation of the zinc dipping solution is as follows: aluminum zinc deposition agent W-2000: 500-550 ml/L; pure water class B H2O: and (4) the balance.
5. The ultra-thick high-phosphorus chemical nickel plating and stabilizing treatment process for the aluminum-based silicon carbide composite material according to claim 1, is characterized in that: in the step 4), the formula of the gloss treatment solution is as follows: 40% nitric acid HNO3：ρ＝1.42g/cm3(ii) a Hydrofluoric acid (HF): rho is 1.12g/cm3，20ml/L。
6. The ultra-thick high-phosphorus chemical nickel plating and stabilizing treatment process for the aluminum-based silicon carbide composite material according to claim 1, is characterized in that: in the step 6), the formula of the pre-plating chemical nickel solution is as follows: ni ion Ni2+Adding in the form of basic nickel carbonate: 5.6-6.4 g/L; sodium hypophosphite NaH2PO2·3H2O：21～27g/L。
7. The aluminum-based silicon carbide composite material of claim 1, having an ultra-thick heightThe phosphorus chemical nickel plating and stabilizing treatment process is characterized in that: in the step 7), the formula of the high-phosphorus chemical nickel plating solution is as follows: ni ion Ni2+Adding in the form of nickel sulfate: 5.0 to 6.2g/L, sodium hypophosphite NaH2PO2·3H2O: 26-33 g/L; the pH value of the high-phosphorus chemical nickel plating solution is tested by adopting a calibrated acidimeter, the test solution is measured after being cooled to room temperature, nickel sulfate is analyzed and supplemented at any time in the plating process according to the loading amount, and the plating solution is supplemented regularly to keep the pH value relatively stable; circularly filtering the high-phosphorus chemical nickel plating solution by using a chemical nickel plating filter with the filtering precision not lower than 5 mu m, wherein the circulating filtering frequency is 7-10 times/h, and the cleaning of the bath solution is ensured; the heating mode of the high-phosphorus chemical nickel plating solution adopts a stainless steel electric heating tube coated by polytetrafluoroethylene, and is provided with a Pt100 temperature control induction probe, the temperature control precision is +/-0.5 ℃, and the heating reliability and the temperature uniformity are ensured.
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