CN116676647A - Preparation method of reinforced nickel coating - Google Patents
Preparation method of reinforced nickel coating Download PDFInfo
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- CN116676647A CN116676647A CN202310675195.9A CN202310675195A CN116676647A CN 116676647 A CN116676647 A CN 116676647A CN 202310675195 A CN202310675195 A CN 202310675195A CN 116676647 A CN116676647 A CN 116676647A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 94
- 238000000576 coating method Methods 0.000 title claims abstract description 89
- 239000011248 coating agent Substances 0.000 title claims abstract description 76
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 54
- 239000002131 composite material Substances 0.000 claims abstract description 41
- VMWYVTOHEQQZHQ-UHFFFAOYSA-N methylidynenickel Chemical compound [Ni]#[C] VMWYVTOHEQQZHQ-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000004070 electrodeposition Methods 0.000 claims abstract description 25
- 238000007747 plating Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000009713 electroplating Methods 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 229910001369 Brass Inorganic materials 0.000 claims description 13
- 239000010951 brass Substances 0.000 claims description 13
- 238000005406 washing Methods 0.000 claims description 13
- 230000004913 activation Effects 0.000 claims description 12
- 230000003213 activating effect Effects 0.000 claims description 10
- 239000002904 solvent Substances 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 239000003513 alkali Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- 238000004140 cleaning Methods 0.000 claims description 5
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 4
- 229910052802 copper Inorganic materials 0.000 claims description 4
- 239000010949 copper Substances 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 241000080590 Niso Species 0.000 claims description 3
- 238000009499 grossing Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229910000838 Al alloy Inorganic materials 0.000 claims description 2
- 229910000975 Carbon steel Inorganic materials 0.000 claims description 2
- 239000010962 carbon steel Substances 0.000 claims description 2
- 238000000151 deposition Methods 0.000 claims description 2
- 230000008021 deposition Effects 0.000 claims description 2
- 238000005260 corrosion Methods 0.000 abstract description 13
- 230000007797 corrosion Effects 0.000 abstract description 11
- 239000003792 electrolyte Substances 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 41
- 238000012360 testing method Methods 0.000 description 13
- 238000005299 abrasion Methods 0.000 description 9
- 238000001994 activation Methods 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 239000000843 powder Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 6
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000002114 nanocomposite Substances 0.000 description 5
- VDJWXZGFYXVVJK-UHFFFAOYSA-N [P].[Ni].[C] Chemical compound [P].[Ni].[C] VDJWXZGFYXVVJK-UHFFFAOYSA-N 0.000 description 4
- 238000012876 topography Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005498 polishing Methods 0.000 description 3
- 238000005728 strengthening Methods 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- OFNHPGDEEMZPFG-UHFFFAOYSA-N phosphanylidynenickel Chemical compound [P].[Ni] OFNHPGDEEMZPFG-UHFFFAOYSA-N 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 231100000241 scar Toxicity 0.000 description 2
- 241000270722 Crocodylidae Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 240000001549 Ipomoea eriocarpa Species 0.000 description 1
- 235000005146 Ipomoea eriocarpa Nutrition 0.000 description 1
- 244000137852 Petrea volubilis Species 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011852 carbon nanoparticle Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- LNNWVNGFPYWNQE-GMIGKAJZSA-N desomorphine Chemical compound C1C2=CC=C(O)C3=C2[C@]24CCN(C)[C@H]1[C@@H]2CCC[C@@H]4O3 LNNWVNGFPYWNQE-GMIGKAJZSA-N 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910021392 nanocarbon Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000012744 reinforcing agent Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/18—Electroplating using modulated, pulsed or reversing current
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/12—Electroplating: Baths therefor from solutions of nickel or cobalt
-
- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electroplating Methods And Accessories (AREA)
Abstract
The invention discloses a preparation method of a reinforced nickel coating, which comprises the following steps: (1) pretreating a sample; (2) Dropwise adding carbon sol into the electroplating solution under the conditions of heating and stirring the electroplating solution to obtain nickel-carbon composite electrodeposition plating solution; (3) Immersing the pretreated sample serving as a cathode and a nickel plate serving as an anode into a nickel-carbon composite electrodeposition plating solution, wherein the positive electrode of a pulse power supply is connected with the anode, the negative electrode is connected with the cathode, and the two electrodes are parallel and opposite to each other for pulse electrodeposition; according to the method, the strength, the wear resistance and the corrosion resistance of the nickel coating are improved by introducing carbon sol into the electrolyte and adopting a pulse electrodeposition method.
Description
Technical Field
The invention relates to a preparation method of a nickel coating, in particular to a preparation method of a reinforced nickel coating.
Background
Nickel coatings are often used in industrial applications due to their good corrosion and wear resistance properties. However, in order to reduce the cost and simplify the process and enhance the comprehensive performance of the coating, the nickel coating is often co-deposited with hard particles to form a high-performance composite coating.
The nickel composite coating uses micron-sized hard particles as a reinforcing agent of the coating, and with the progress of industry, the preparation process of the composite coating cannot meet the current pursuit of higher-performance coatings. Nanoparticle-reinforced composite coatings have higher hardness, strength, and abrasion resistance than microparticle-reinforced composite coatings, and thus nanocomposite coatings have become a hot spot of research in recent years. In the existing process, particles such as SiC, graphite powder and the like are directly added into the electroplating solution to realize the purpose of composite electrodeposition. The process has the phenomenon that graphite particles are easy to agglomerate, the dispersion strengthening effect is difficult to achieve, and the obtained composite coating has poor strength and wear resistance.
Disclosure of Invention
The invention aims to: the invention aims to provide a preparation method of a reinforced nickel coating for improving the strength, wear resistance and corrosion resistance of the nickel coating.
The technical scheme is as follows: the preparation method of the reinforced nickel coating comprises the following steps:
(1) Pretreating a sample;
(2) Dropwise adding carbon sol into the electroplating solution under the conditions of heating and stirring the electroplating solution to obtain nickel-carbon composite electrodeposition plating solution;
(3) And immersing the pretreated sample serving as a cathode and a nickel plate serving as an anode in a nickel-carbon composite electrodeposition plating solution, wherein the positive electrode of a pulse power supply is connected with the anode, the negative electrode is connected with the cathode, and the two electrodes are parallel and opposite to each other for pulse electrodeposition.
Preferably, in the step (2), the carbon sol content in the composite electrodeposition plating solution is 10-40 mL/L, wherein the carbon sol concentration is 0.01-0.03 g/L.
The carbon sol has good dispersion performance, good conductivity and self-lubricating performance, the composite coating formed by the carbon nano particles and other metals can improve the related mechanical properties of the coating, the addition of the carbon particles can refine grains, and the hardness and strength can also be improved; in addition, the nano carbon particles with high-efficiency self-lubricating effect can greatly improve the friction and wear resistance of the coating.
The carbon sol is HNO with the concentration of 0.1-0.2M 3 ，0.1～0.2M(CH 2 OH) 2 And 0.1 to 2g/L of C 12 H 25 SO 4 And (3) electrolyzing Na to obtain the catalyst.
Preferably, the pulse electrodeposition parameters are: the current density is 30-50 mA/cm 2 The duty ratio is 60-80%, the frequency is 500-1500 Hz, and the deposition time is 20-40 minutes. Compared with the common direct current deposition process, the pulse electrodeposition process has more excellent surface brightness, abrasion resistance, corrosion resistance, high conductivity and other performances, can obtain a noble metal coating with higher quality, thin and uniform thickness, and can greatly save the production cost.
Preferably, in step (2), the plating solution includes: 140-160 g/L NiSO 4 Particles, 12-18 g/L NH 4 Cl、15～20g/L H 3 BO 3 And 0.2 to 1g/L C 12 H 25 SO 4 Na, water as solvent.
Preferably, in the step (1), the sample is brass, pure copper, carbon steel, an aluminum alloy, or the like. The sample was prepared into a 15mm by 20mm specification sample using a cutter or scissors to be applied to a plating bath apparatus.
Preferably, in the step (1), the pretreatment of the sample includes a surface smoothing treatment, an alkali washing treatment and an activation treatment
Preferably, the smoothing process is: and (3) pasting insulating glue on the surface of the sample, exposing an exposed surface with a certain area, polishing the exposed surface from thick to thin by using sand paper with different mesh numbers, and finally cleaning the sample by using deionized water and drying for later use.
Preferably, in the alkaline washing step two, the alkaline washing liquid comprises the following components: 35-60 g/L NaOH and 8-13 g/L NaH 2 PO 4 ·H 2 O, water is the solvent. And (5) washing the sample with deionized water after the alkaline washing is completed for 10 min.
Preferably, the activation treatment is: the sample cathode, stainless steel plate as anode, immerse the cathode and anode in activating solution, the positive pole of DC power source connects with anode, the negative pole connects with cathode, the two electrodes are parallel and opposite to each other, and activating treatment is carried out in constant current mode.
Preferably, the activating solution comprises 15-25 g/LC 6 H 8 O 7 And 60 to 70g/L C 6 H 5 O 7 (NH 4 ) 3 Water is the solvent.
Preferably, in the activation treatment, the current density is 30-40 mA/cm 2 The activation time was 90 seconds.
The beneficial effects are that: compared with the prior art, the invention has the following remarkable advantages: (1) According to the method, the strength, the wear resistance and the corrosion resistance of the nickel coating are improved by introducing carbon sol into the electrolyte and adopting a pulse electrodeposition method; (2) The addition amount of the carbon sol with 15ML/L concentration of 0.025g/L reaches the maximum value of 420HV, and the corrosion rate is 7.11 multiplied by 10 -3 The wear amount of mm/year is reduced by 44.9 percent compared with that of the method without adding carbon sol; (3) The device for preparing the nickel-phosphorus-carbon nano composite coating is simple and the manufacturing process is simple: the equipment only needs an electroplating pool, a direct current power supply, wires, clamps and the like, so that the cost is low; the common chemical reagent required by electroplating has wide market selling sources, so that the plating method is suitable for mass industrial production; (4) The nickel-phosphorus plating solution of the plating solution used in the method can be stored for a long time, and the chemical reagent used in the plating has little pollution to the environment; (5) The stainless steel plate used for activation is taken as an anode, has great inertia, and does not generate new substances to be polluted in the reactionThe dyeing activating liquid can be reused for many times.
Drawings
FIG. 1 is a scan of the surface topography prepared in example 1, comparative example 2; wherein, figure (a) is a pure nickel coating of comparative example 1; FIG. (b) is a nickel carbon composite coating of example 1 with 15mL/L carbon sol added; FIG. (c) is a nickel carbon composite coating of comparative example 2 with 50mL/L carbon sol added;
FIG. 2 is a cross-sectional topography scan of the pure nickel and nickel carbon composite coatings prepared in example 1, comparative example 2; wherein, figure (a) is a pure nickel coating of comparative example 1; FIG. (b) is a nickel carbon composite coating of example 1 with 15mL/L carbon sol added; FIG. (c) is a nickel carbon composite coating of comparative example 2 with 50mL/L carbon sol added;
FIG. 3 is a XRD pattern and a grain size comparison pattern of the pure nickel and nickel carbon composite coatings prepared in example 1, comparative example 1, and comparative example 2; wherein, figure (a) is the XRD pattern of the pure nickel and nickel carbon composite coating; graph (b) is a graph of average grain size comparison for a pure nickel and nickel carbon composite coating;
fig. 4 is a chart showing the surface morphology of the friction wear scar and a scan of the cross section of the wear scar for the pure nickel and nickel carbon composite coatings prepared in example 1, comparative example 1, and comparative example 2. Wherein, figure (a) is a comparative example pure nickel coating; FIG. (b) is a nickel carbon composite coating of example 1 with 15mL/L carbon sol added; FIG. (c) is a nickel carbon composite coating of comparative example 2 with 50mL/L carbon sol added;
FIG. 5 is a graph showing the hardness of the pure nickel and nickel carbon composite coatings prepared in examples 1 to 5, comparative example 1, comparative example 2;
fig. 6 is a graph comparing polarization curves of pure nickel and nickel carbon composite coatings prepared in example 1, comparative example 1, and comparative example 2.
Detailed Description
The technical scheme of the invention is further described below by referring to examples.
Example 1
The preparation method of the reinforced nickel coating comprises the following steps:
(1) Pretreatment of the sample
Polishing: the method comprises the steps of preparing an H62 brass sheet with the thickness of 1mm into a sample with the specification of 15mm multiplied by 20mm by using a cutting machine or scissors so as to be suitable for a plating bath device, attaching insulating glue on one surface of the brass sheet sample, sequentially polishing the other exposed surface by using 800# abrasive paper, 1000# abrasive paper, 1500# abrasive paper and 2000# abrasive paper according to the sequence from thick to thin, and then cleaning by using deionized water;
alkali washing: placing the polished brass sample into alkali washing liquid at 75 ℃ for alkali washing for 10min, and washing the sample with deionized water after the alkali washing is finished; specifically, the alkali washing liquid comprises the following components: 10g NaOH powder and 2g NaH 2 PO 4 ·H 2 O powder is used as solute, 188mL of deionized water is used as solvent;
activating: clamping the alkali washed brass sample on a fixed fixture as a cathode, taking a stainless steel plate with the specification of 40mm multiplied by 3mm as an anode, immersing a cathode and an anode in an activating solution, connecting the anode with a direct current power supply, connecting the cathode with the anode, and arranging the two electrodes in parallel and opposite to each other, wherein the current density is 30mA/cm 2 The brass sample is subjected to activation treatment in a constant-current mode, the activation time is 90s, and the whole activation process is carried out at room temperature. Taking out the brass sample after activation, cleaning with deionized water and drying; specifically, the composition of the activating solution is as follows: 5g C 6 H 8 O 7 Powder sum 13g C 6 H 5 O 7 (NH 4 ) 3 The powder was solute and 182mL deionized water was solvent.
(2) Nickel-carbon composite electro-deposition plating solution preparation
The preparation of the carbon sol comprises the following steps:
step one, preparing electrolyte with the concentration of 0.1M HNO 3 、0.1M(CH 2 OH) 2 And 0.5g/L C 12 H 25 SO 4 Na is solute, and the solvent is water;
and secondly, taking two high-purity graphite plates with the specification of 100mm multiplied by 50mm multiplied by 3mm as electrodes, fixing the two graphite plates by using crocodile clips with pure copper bars, immersing the two graphite plates in electrolyte, and fixing the two graphite plates in parallel and relatively. The whole electricity isThe pool removing device is arranged in an ultrasonic instrument with the vibration frequency of 40KHz, the ultrasonic instrument is started, the anode and the cathode of a direct current power supply are respectively connected with copper bars, a constant current mode of the direct current power supply is set, and the current density is 5mA/cm 2 The carbon sol is obtained after 22 hours of electrolytic reaction, and the concentration is 0.025g/L.
Heating and stirring the plating solution by using a magnetic stirrer under the reaction conditions of 300r/min and 60 ℃ and slowly dripping carbon sol into the plating solution to obtain nickel-carbon composite electrodeposition plating solution; the composition of the electroplating solution is as follows: 30g NiSO 4 Particles, 3g NH 4 Cl powder, 3g H 3 BO 3 Powder and 0.1. 0.1g C 12 H 25 SO 4 Na powder is taken as solute, 164mL of deionized water is taken as solvent, and 15mL of carbon sol is added after the plating solution is fully dissolved.
(3) Clamping the treated brass sample on a fixed fixture to serve as a cathode, taking a high-purity nickel plate with the specification of 40mm multiplied by 3mm and the purity of more than or equal to 99.9% as an anode, immersing a cathode and an anode in electroplating liquid, connecting the anode of a pulse power supply with the anode nickel plate, connecting the cathode with the cathode brass sample, mutually parallel and opposite two electrodes, and setting pulse electrodeposition parameters: current density 40mA/cm 2 Duty cycle 75%, frequency 1000Hz. Starting a pulse power switch to perform electrodeposition, wherein the electrodeposition time is 30min; and (3) taking out the brass sample in the step four, washing the brass sample by using deionized water, and drying the brass sample to obtain the nickel-carbon composite coating added with 15mL/L of carbon sol.
Example 2
Based on example 1, the addition amount of the carbon sol was changed to 10mL/L, and the other conditions were unchanged.
Example 3
Based on example 1, the addition amount of the carbon sol was changed to 20mL/L, and the other conditions were unchanged.
Example 4
Based on example 1, the addition amount of the carbon sol was changed to 30mL/L, and the other conditions were unchanged.
Example 5
Based on example 1, the addition amount of the carbon sol was changed to 40mL/L, and the other conditions were unchanged.
Comparative example 1
On the basis of example 1, no carbon sol was added, and the remaining conditions were unchanged.
Comparative example 2
Based on example 1, the addition amount of the carbon sol was changed to 50mL/L, and the other conditions were unchanged.
Microstructure characterization and phase testing:
as shown in fig. 1, which shows the surface topography of the embodiment example 1 (fig. 1 b), the comparative example 1 (fig. 1 a) and the comparative example 2 (fig. 1 c), the surface topography of the pure nickel coating of the comparative example 1 and the nickel-carbon composite coating of the embodiment example 1 are both small protrusion structures. Example 1 the surface of a pure nickel coating added with 15mL/L carbon sol was finer and smoother than the pure nickel coating, which was mainly due to the addition of carbon particles to refine the grains. However, as the amount of carbon sol added increases, the surface of the coating of comparative example 2 becomes more rough because too much carbon sol promotes the hydrogen evolution reaction during electrodeposition, resulting in a change in the surface morphology.
As shown in fig. 2, which is the sectional morphology of the embodiment examples 1 (fig. 2 b), 1 (fig. 2 a) and 2 (fig. 2 c), it can be seen from the figures (2 a) and (2 b) that the nickel-carbon composite coating to which the carbon sol is added becomes thicker as the addition amount of the carbon sol increases, because the addition of the carbon particles is advantageous for improving the electrodeposition efficiency thereof. As can be seen from fig. 2c, the nickel carbon composite coating thickness is reduced because excessive carbon particles may cause an increased probability of agglomeration thereof, which may reduce the efficiency of electrodeposition.
As can be seen from the XRD comparison patterns and average grain size comparison patterns of example 1 and comparative example 1, comparative example 2 of fig. 3, the addition of carbon particles does not change the phase of the coating. From the XRD patterns of example 1 and comparative examples 1 and 2, the average grain size of the coating was calculated using the scherrer equation, and the comparison result revealed that the average grain size of example 1 was the smallest. This demonstrates that the addition of carbon particles can refine the grain size of the pulsed electrodeposited nickel coating, lateral elucidation of the strengthening mechanism of the coating.
Performance test:
1. abrasion resistance test
The nickel-carbon composite coating in example 1, and the coatings in comparative examples 1 and 2 were subjected to wear resistance testing using an HSR-2M type high-speed reciprocating frictional wear testing machine. The test adopts zirconia hard pellets with the diameter of 4mm, 500g is applied and rubbed back and forth on the surface of the coating for 10min, and finally the grinding mark is obtained. And photographing and measuring the abrasion marks by using a 3D video microscope to obtain the abrasion cross-section morphology of the pure nickel coating and the nickel-carbon composite coating, wherein the test result is shown in figure 4.
FIG. 4a is a pure nickel coating of comparative example 1; FIG. (b) is a nickel carbon composite coating of example 1 with 15mL/L carbon sol added; FIG. 2 shows the nickel-carbon composite coating added with 50mL/L carbon sol of comparative example 2, from which the abrasion loss of comparative example 1, example 1 and comparative example 2 was 7.52X10, respectively -4 mm 3 、4.14×10 -4 mm 3 、6.17×10 -4 mm 3 . The abrasion loss of the nickel-carbon composite coating added with 15mL/L carbon sol in example 1 is minimum, and compared with the abrasion loss of the pure nickel coating in comparative example 1, the abrasion loss of the pure nickel coating is reduced by 44.9%. Therefore, the wear resistance of the nickel-phosphorus coating can be effectively improved by adding a proper amount of carbon particles, but the thickness of the nickel-phosphorus-carbon nano composite coating added with excessive carbon sol is reduced, and the wear resistance is reduced.
2. Hardness test
The hardness test was performed on the coatings of examples 1-5, comparative example 1 and comparative example 2 using a HXS-1000TAC semi-automatic durometer. The test uses 300g load to test the coating, including loading 10s, keeping 15s, unloading 15s, to obtain a diamond print, and the Vickers hardness value of the coating is obtained through measurement and calculation, and the test result is shown in figure 5.
As can be seen from FIG. 5, the hardness of the nickel-phosphorus-carbon nanocomposite coating layer increased as the concentration of the carbon sol added gradually increased, and the hardness of comparative example 1, examples 1 to 5, and comparative example 2 were 314HV, 420HV, 396HV, 380HV, 368HV, and 364HV, respectively. When the concentration of the added carbon sol reaches 15mL/L, the hardness reaches the maximum value of 420HV, and when the carbon sol with higher concentration is added, the hardness of the nickel-phosphorus-carbon nano composite coating is obviously reduced. This is because when a proper amount of carbon sol is added, the addition of carbon particles increases nucleation sites in the process of electric crystallization, so that the grains of the coating are refined, the hardness of the coating is enhanced, and when excessive carbon particles are added, the grains of the coating are coarse, so that the fine-grain strengthening effect is not outstanding.
3. Corrosion resistance test
Corrosion electrochemical tests were performed on example 1, comparative example 1 and comparative example 2 using a morning glory electrochemical workstation. The open circuit potential and polarization curve of the coatings were tested in 3.5wt% NaCl solution using saturated calomel electrode and platinum electrode, respectively, with example 1, comparative example 1 and comparative example 2. The test results are shown in fig. 6.
As can be seen from FIG. 6, the corrosion rates of comparative example 1, example 1 and comparative example 2 were 1.11X10, respectively -2 mm/year、7.11×10 -3 mm/year、1.06×10 -2 mm/year. This result shows that the addition of carbon particles can effectively improve the corrosion resistance of the coating. The best corrosion resistance of the nickel carbon composite coating prepared by adding 15mL/L carbon sol is demonstrated by the most positive self-corrosion potential and the least self-corrosion current density of example 1.
Claims (10)
1. The preparation method of the reinforced nickel coating is characterized by comprising the following steps of:
(1) Pretreating a sample;
(2) Dropwise adding carbon sol into the electroplating solution under the conditions of heating and stirring the electroplating solution to obtain nickel-carbon composite electrodeposition plating solution;
(3) And immersing the pretreated sample serving as a cathode and a nickel plate serving as an anode in a nickel-carbon composite electrodeposition plating solution, wherein the positive electrode of a pulse power supply is connected with the anode, the negative electrode is connected with the cathode, and the two electrodes are parallel and opposite to each other for pulse electrodeposition.
2. The method for producing a strengthened nickel coating according to claim 1, wherein in step (2), the carbon sol content in the composite electrodeposition bath is 10 to 40mL/L, and wherein the carbon sol concentration is 0.01 to 0.03g/L.
3. The strengthened nickel coating according to claim 1The preparation method is characterized in that in the step (3), the pulse electrodeposition parameters are as follows: the current density is 30-50 mA/cm 2 The duty ratio is 60-80%, the frequency is 500-1500 Hz, and the deposition time is 20-40 minutes.
4. The method of producing a strengthened nickel coating according to claim 1, wherein in step (2), the plating solution comprises: 140-160 g/L NiSO 4 Particles, 12-18 g/L NH 4 Cl、15～20g/L H 3 BO 3 And 0.2 to 1g/LC 12 H 25 SO 4 Na, water as solvent.
5. The method of producing a strengthened nickel coating according to claim 1, wherein in step (1), the sample is brass, pure copper, carbon steel or an aluminum alloy.
6. The method for producing a reinforced nickel coating according to claim 1, wherein in the step (1), the pretreatment of the sample comprises a surface smoothing treatment, an alkali washing treatment and an activation treatment.
7. The method for producing a strengthened nickel coating according to claim 6, wherein the alkaline cleaning solution in the alkaline cleaning step two has the composition: 35-60 g/L NaOH and 8-13 g/L NaH 2 PO 4 ·H 2 O, water is the solvent.
8. The method of producing a strengthened nickel coating according to claim 6, wherein the activation treatment is: the sample cathode, stainless steel plate as anode, immerse the cathode and anode in activating solution, the positive pole of DC power source connects with anode, the negative pole connects with cathode, the two electrodes are parallel and opposite to each other, and activating treatment is carried out in constant current mode.
9. The method for producing a reinforced nickel coating according to claim 8, wherein the activating solution contains 15 to 25g/L C 6 H 8 O 7 And 60 to 70g/L C 6 H 5 O 7 (NH 4 ) 3 Water is the solvent.
10. The method for producing a reinforced nickel coating according to claim 8, wherein the current density in the activation treatment is 30 to 40mA/cm 2 The activation time is 60-120 seconds.
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