CN118292063A - Device and method for preparing nanocrystalline nickel coating by dynamic flexible friction-assisted jet flow electrodeposition - Google Patents
Device and method for preparing nanocrystalline nickel coating by dynamic flexible friction-assisted jet flow electrodeposition Download PDFInfo
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 238000004070 electrodeposition Methods 0.000 title claims abstract description 44
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 44
- 238000000576 coating method Methods 0.000 title claims abstract description 33
- 239000011248 coating agent Substances 0.000 title claims abstract description 32
- 238000000034 method Methods 0.000 title claims abstract description 28
- 238000007747 plating Methods 0.000 claims abstract description 47
- 230000007246 mechanism Effects 0.000 claims description 54
- 230000005540 biological transmission Effects 0.000 claims description 22
- 238000000151 deposition Methods 0.000 claims description 17
- 230000008021 deposition Effects 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 238000009713 electroplating Methods 0.000 claims description 11
- 238000001540 jet deposition Methods 0.000 claims description 11
- 239000000758 substrate Substances 0.000 claims description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 239000000463 material Substances 0.000 claims description 6
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims description 5
- 239000004327 boric acid Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- LAIZPRYFQUWUBN-UHFFFAOYSA-L nickel chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Ni+2] LAIZPRYFQUWUBN-UHFFFAOYSA-L 0.000 claims description 5
- RRIWRJBSCGCBID-UHFFFAOYSA-L nickel sulfate hexahydrate Chemical compound O.O.O.O.O.O.[Ni+2].[O-]S([O-])(=O)=O RRIWRJBSCGCBID-UHFFFAOYSA-L 0.000 claims description 5
- 229940116202 nickel sulfate hexahydrate Drugs 0.000 claims description 5
- 230000001360 synchronised effect Effects 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011324 bead Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000007921 spray Substances 0.000 claims description 4
- 244000137852 Petrea volubilis Species 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 125000004122 cyclic group Chemical group 0.000 claims 1
- 230000000694 effects Effects 0.000 abstract description 10
- 239000001257 hydrogen Substances 0.000 abstract description 6
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000007670 refining Methods 0.000 abstract description 2
- 238000005498 polishing Methods 0.000 description 8
- 239000007769 metal material Substances 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- 230000007547 defect Effects 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229910052782 aluminium Inorganic materials 0.000 description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000011010 flushing procedure Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
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- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002707 nanocrystalline material Substances 0.000 description 2
- 230000024121 nodulation Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
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- 238000009423 ventilation Methods 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
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- 239000000835 fiber Substances 0.000 description 1
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- 150000002431 hydrogen Chemical class 0.000 description 1
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- 230000010287 polarization Effects 0.000 description 1
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- CVHZOJJKTDOEJC-UHFFFAOYSA-N saccharin Chemical compound C1=CC=C2C(=O)NS(=O)(=O)C2=C1 CVHZOJJKTDOEJC-UHFFFAOYSA-N 0.000 description 1
- 229940081974 saccharin Drugs 0.000 description 1
- 235000019204 saccharin Nutrition 0.000 description 1
- 239000000901 saccharin and its Na,K and Ca salt Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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Abstract
The invention discloses a device and a method for preparing a nanocrystalline nickel coating by dynamic and flexible friction-assisted jet flow electrodeposition, which belong to the field of jet flow electrodeposition and mainly have the function of efficiently preparing a high-quality nickel coating with nanocrystalline grain size. The invention designs a novel jet flow electrodeposition technology assisted by dynamic flexible rotary friction, and is matched with a dynamic flexible rotary friction device on the basis of jet flow electrodeposition, and periodically rotates in the electrodeposition process to flexibly rub the surface of an electrodeposited cathode, thereby achieving the effects of leveling a plating layer, removing hydrogen and impurities and refining grains and finally obtaining a high-quality nanocrystalline nickel plating layer.
Description
Technical Field
The invention belongs to the field of jet flow deposition, and particularly relates to a device and a method for preparing a nanocrystalline nickel coating by dynamic and flexible friction-assisted jet flow deposition.
Background
Compared with the common metal material, the nanocrystalline metal material has obviously improved strength and hardness, better plastic toughness, strong corrosion resistance and better comprehensive mechanical property, and therefore, the preparation method thereof needs to be studied intensively. The traditional manufacturing method of nanocrystalline metal materials, such as external pressure synthesis methods, has the defects of higher cost, high process requirement, higher porosity of finished products and the like.
At present, researchers turn to the field of electrodeposition to manufacture nanocrystalline materials, and the nanocrystalline materials obtained by jet electrodeposition processing have the advantages of low porosity of an electrodeposited layer, better quality, lower cost and higher efficiency, and are the most ideal method for manufacturing nanocrystalline metal materials. However, the pure jet electrodeposition method has certain defects, such as the influence of electroplating solution impurities on the material of a deposited layer, coating bulges generated by uneven jet flow, unavoidable cathodic hydrogen evolution phenomenon and the like. Through a great deal of researches, the defects existing in the jet flow deposition can be effectively relieved by using a friction auxiliary method, the jet flow deposition mainly comprises hard friction, sheath friction and the like, the hard friction uses rigid materials for hard friction, the effects of grain refinement and coating leveling are excellent, but the abrasion is serious; the sheath friction is electrodeposited by adopting a brush plating mode, but the method is mostly manually repaired at present, automation is not realized, and although the effect of solving the hydrogen evolution phenomenon is good, the uneven interelectrode gap and the softer friction pair lead to the fact that the larger bulges on the deposition layer are difficult to remove, and the leveling effect is poor.
In recent years, a flexible friction mode is researched and invented, and flexible materials with certain strength and toughness are adopted for friction, such as biological bristles, natural fibers and the like, and the method has the comprehensive advantages of hard friction and sheath friction, can realize the effects of leveling a coating, removing hydrogen, removing impurities, refining grains and the like, and remarkably improves the comprehensive performance of a deposition layer. However, the method is started later and is mostly applied to bath plating, and the field of jet electrodeposition has little development.
Disclosure of Invention
The invention provides a device and a method for preparing a nanocrystalline nickel coating by dynamic flexible friction-assisted jet flow deposition, which are based on a jet flow electrodeposition technology, wherein a dynamic flexible friction device capable of automatically rotating is additionally arranged in a self-grinding way, the comprehensive mechanical property and the surface quality of the nanocrystalline nickel coating are obviously improved, the limiting current density is improved, the rapid preparation of a high-quality nanocrystalline nickel coating metal material can be realized, and the problems in the prior art are solved.
A method for preparing a nanocrystalline nickel coating by dynamic flexible friction-assisted jet electrodeposition comprises the following steps:
Step 1, providing a conductive workpiece cathode substrate, polishing the surface of the workpiece cathode substrate, cleaning with deionized water and alcohol, and drying for later use;
Step 2, preparing a plating solution: heating deionized water to a certain temperature, adding boric acid, and then sequentially adding nickel sulfate hexahydrate and nickel chloride hexahydrate as nickel element sources;
Step 3, fully mixing the plating solution: stirring and mixing the solution obtained in the step 2, and simultaneously adding dilute hydrochloric acid with a certain concentration to maintain the pH range of the solution;
Step 4, preparing jet equipment: the flexible brush is replaced by the flexible rotary friction auxiliary equipment, a sufficient amount of nickel beads are added into the anode cavity, and the flexible friction auxiliary jet electrodeposition is carried out in the subsequent steps;
step 5, cathode workpiece installation: clamping the cathode substrate obtained in the step 1 onto a jet electrodeposition workbench;
Step 6, jet deposition: the electroplating solution obtained in the step 3 is added into a plating solution tank of a plating solution circulating mechanism 5 in a dynamic and flexible rotary friction auxiliary jet flow deposition device, a water pump in the tank is electrified, and an X-axis transmission mechanism 3 and a friction auxiliary mechanism 4 are electrified, so that a nozzle reciprocates at a certain scanning speed, and a brush rotates at a low speed to assist jet flow deposition work through flexible friction;
step 7, soaking and flushing the workpiece: soaking the cathode workpiece after the plating layer is obtained in the step 6 in distilled water, and then flushing the cathode workpiece with distilled water for a plurality of times to remove residual electroplating liquid on the surface of the plating layer;
step 8, integrally drying the workpiece: and (3) naturally air-drying the cathode workpiece after the plating layer obtained in the step (7) at a ventilation position.
In the steps, the cathode substrate used in the step 1 is made of metal or graphite, metallographic sand paper is adopted for rough polishing before the substrate is cleaned, then a metallographic polishing machine is adopted for fine polishing, and deionized water, alcohol, acetone and the like are adopted for cleaning and drying during the substrate pretreatment;
In the step 2, the temperature is 80-100 ℃, the adding amount of boric acid is 20-60 g/L, the adding amount of nickel sulfate hexahydrate is 240-280 g/L, and the adding amount of nickel chloride hexahydrate is 20-60 g/L;
step 3, adding hydrochloric acid with the concentration range of 10 wt% -20: 20 wt% and keeping the pH range of the solution to be 3.8-4.2;
The flexible brush material adopted in the step 4 is bristle, and the diameter of nickel beads is within 5-10 mm;
in the step 5, the workpiece adopts dilute hydrochloric acid in the same step 3 to perform certain activation treatment on the surface of the workpiece;
The specific parameters of jet electrodeposition in the step 6 are as follows: the temperature of the electroplating solution is kept at 35-55 ℃, the current density is controlled within 150-350A/dm 2, the scanning speed is 300-1200 mm/min, the deposition time is 40-80 min, the nozzle flow is 200-300L/h, the rotating friction rotating speed is 0-8 r/min, and the interelectrode gap is 1-2 mm.
The dynamic flexible rotary friction auxiliary jet flow deposition device used in the method comprises the following steps: a frame mechanism 1, a Z-axis transmission mechanism 2, an X-axis transmission mechanism 3, a rotary friction mechanism 4 and a plating solution circulation mechanism 5; the frame mechanism 1 bears the weight of each part and divides each part, the X-axis transmission mechanism 3 enables the anode nozzle to reciprocate and circularly scan, the Z-axis transmission mechanism 2 controls the gap between electrodes, the rotary friction mechanism 4 enables the brush to flexibly rotate and rub the cathode surface to improve the jet electrodeposition quality, and the plating solution circulation mechanism 5 circularly sprays to enable the plating solution of the jet electrodeposition to flow to obtain original power;
The rotary friction mechanism 4 is characterized in that an anode cavity 409 is fixed through an anode connecting piece 408, a fixed bearing 407 is arranged on the anode cavity, a rotary driven wheel 406 is arranged on the outer ring of the bearing, a brush wheel 405 is arranged below the driven wheel, and a nozzle 404 is arranged at the bottom of the anode cavity; the side of the anode connecting piece is provided with a motor 401, and the motor is provided with a driving wheel 402. When the jet electro-deposition device works, the motor 401 is electrified, the matched driving wheel 402 is rotated, the driven wheel 406 is driven by the synchronous belt to rotate according to a certain transmission ratio, the matched brush wheel 405 is rotated, the flexible brush on the driven wheel is driven to rotate and rub the surface of the cathode workpiece 403, and high-quality jet electro-deposition is realized.
The beneficial effects are that: the invention provides a device and a method for preparing a nanocrystalline nickel coating by dynamic and flexible friction-assisted jet deposition, which have the following advantages compared with the prior art:
1. According to the invention, on the basis of the original jet electrodeposition equipment for preparing the nanocrystalline nickel coating, the dynamic flexible rotary friction auxiliary device is independently designed and added, and the dynamic flexible rotary friction is continuously carried out on the electrodeposited coating in the process of preparation, so that the effects of coating leveling, hydrogen removal, impurity removal and grain refinement are achieved, and finally the high-quality nanocrystalline nickel coating is obtained; compared with the common jet electrodeposition, the method can effectively remove hydrogen and impurities in the electrodeposition process, and planarize the deposition surface, so that the grain size distribution is more uniform and finer, and the hardness and the surface quality of a plating layer can be greatly improved;
2. According to the invention, by adding the dynamic flexible friction auxiliary device and matching with optimal technological parameters of synchronous process experiment, the comprehensive performance of the nickel plating layer is enhanced, the limiting current density is obviously improved, and the high-efficiency and high-quality preparation of the nanocrystalline nickel plating layer is realized.
Drawings
FIG. 1 is a schematic diagram of flexible friction assisted jet electrodeposition layer quality enhancement and nanocrystalline nickel formation promotion in an embodiment of the present invention;
FIG. 2 is a schematic diagram of a dynamic flexible friction assist device assembly;
FIG. 3 is a schematic assembly view of a specific rotary friction portion and a key part view;
FIG. 4 shows the surface topography of a nickel coating deposited at different current densities using dynamic flexible rotary friction assisted jet electrodeposition and friction free jet electrodeposition, wherein a is the friction free and b is the current densities of a/b1 to a/b4 after flexible friction of 150, 250, 300 and 350A/dm 2, respectively;
FIG. 5 is a graph of microhardness (left) and thickness (right) of nickel plating deposited at different current densities using dynamic flexible rotary friction assisted jet electrodeposition and friction free jet electrodeposition;
FIG. 6 shows XRD patterns (left) and grain sizes (right) of nanocrystalline nickel coatings deposited at different current densities using dynamic flexible rotary friction assisted jet electrodeposition and friction free jet electrodeposition;
In the figure, 1-frame mechanism, 2-Z axis transmission mechanism, 3-X axis transmission mechanism, 4-rotary friction mechanism, 5-plating solution circulation mechanism, 401-motor, 402-driving wheel, 403-cathode workpiece, 404-nozzle, 405-brush wheel, 406-driven wheel, 407-fixed bearing, 408-anode connecting piece, 409-anode cavity.
Detailed Description
The invention is described in detail below with reference to the attached drawings and the specific embodiments:
examples
As shown in fig. 2 and 3, a device for preparing nanocrystalline nickel plating by dynamic flexible friction-assisted jet deposition comprises a frame mechanism 1, an X-axis transmission mechanism 3, a Z-axis transmission mechanism 2, a rotary friction mechanism 4 and a plating solution circulation mechanism 5; the main body of the frame mechanism 1 is an aluminum profile, and is connected with each other through built-in bolts so as to bear the weight of each part and divide each part; the main body of the X-axis transmission mechanism 3 is a ball screw sliding table, and is connected with the frame structure 1 through a nut on an aluminum profile on the back of the sliding table in a bolt way, so that the anode nozzle reciprocates and circularly and controls the reciprocating speed; the main body of the Z-axis transmission mechanism 2 is a ball screw sliding table, and is connected with a sliding table of the X-axis transmission mechanism 3 through a nut on an aluminum profile on the back of the sliding table to control the gap between the electrodes; the rotary friction mechanism 4 enables the brush to flexibly rotate and rub the surface of the cathode to improve jet electrodeposition quality, and the plating solution circulating mechanism 5 is connected with the anode cavity of the rotary friction mechanism 4 through a pipeline to spray plating solution in a reciprocating manner;
The rotary friction mechanism 4 includes: motor 401, driving wheel 402, driven wheel 406, nozzle 404, brush wheel 405, driven wheel 406, fixed bearing 407, anode connection 408, anode cavity 409; a fixed bearing 407 is arranged on an anode cavity 409, the anode cavity 409 is fixed through an anode connecting piece 408, the anode connecting piece 408 is positioned above the fixed bearing 407, a nozzle 404 is arranged at the bottom of the anode cavity 409, a cathode workpiece 403 is positioned below the nozzle 404, the anode cavity 409 penetrates through the fixed bearing 407, a driven wheel 406 is arranged on the outer ring of the fixed bearing 407, a brush wheel 405 is arranged below the driven wheel, a motor 401 is arranged on the side edge of the anode connecting piece 408, a driving wheel 402 is arranged on the motor 401, and the driving wheel 402 is connected with the driven wheel 406 through a synchronous belt; the anode connecting piece 408 is integrally arranged on a sliding table of the Z-axis transmission mechanism 2, and the top end of the anode cavity 409 is connected with the plating solution circulating mechanism 5 through a pipeline;
When the device works, the X-axis transmission mechanism 3 enables the anode nozzle to reciprocate and circularly scan, the Z-axis transmission mechanism 2 controls the gap between electrodes, and the plating solution circulation mechanism 5 circularly sprays to enable the plating solution for jet electrodeposition to flow so as to obtain original power; in the rotary friction mechanism 4, a motor 401 is electrified, a driving wheel 402 matched with the motor is rotated, a driven wheel 406 is driven by a synchronous belt to rotate according to a certain transmission ratio, a matched brush wheel 405 is rotated, a flexible brush on the driving wheel is driven to rotate and rub the surface of a cathode workpiece 403, and high-quality jet electrodeposition is realized.
The preparation method of the graphite-based nanocrystalline nickel plating layer by adopting the device comprises the following steps:
step 1, selecting graphite as a cathode substrate material, polishing and polishing step by using metallographic sand paper in #1 to #6, fine polishing by using an electrodeless speed-regulating metallographic polishing machine, and cleaning and drying by using deionized water and alcohol;
Step 2, heating 100 mL deionized water to about 90 ℃, adding boric acid 4g into the mixture, stirring the mixture to serve as a plating solution buffer, sequentially adding nickel sulfate hexahydrate 26 g and nickel chloride hexahydrate 4g serving as a plating solution nickel source, and finally adding saccharin 0.5 g into the mixture to refine grains, and fully stirring the mixture;
step 3, adding hydrochloric acid with the mass fraction of 10% into the electroplating solution obtained in the step 2, and adjusting the pH value of the solution to be 4.0;
Step 4, preparing a nickel coating by adopting a dynamic and flexible rotary friction auxiliary jet flow deposition device as shown in fig. 2, adding the electroplating solution obtained in the step 3 into a plating solution tank, heating the water bath to about 50 ℃, setting the processing parameters to be 1000 mm/min scanning speed, 60min deposition time, 300L/h flow and 1 mm inter-electrode gap, and adjusting the rotating speeds of a driven wheel 405 and a brush wheel 406 in the rotary friction mechanism 4 as shown in fig. 3 to 4 r/min through a motor 401 and a driving wheel 402, wherein the current densities are set to 150, 200, 250, 300, 350A/dm 2;
and 5, soaking each coating obtained in the step 4 in distilled water for 1.5 hours, flushing with distilled water for 3 times, and finally naturally airing at a ventilation position.
And (3) analyzing and testing each performance of the obtained plating layer:
Surface topography analysis: the surface morphology of the sample piece after the plating is observed by using a Zeiss Ultra Plus field emission scanning electron microscope, as shown in figure 4, wherein a is no flexible friction, b is that after flexible friction exists, the current densities of a/b1 to a/b4 are respectively 150, 250, 300 and 350A/dm 2, and the point discharge effect obviously causes the generation of nodulation along with the gradual increase of the current density, and the increment of the deposited nodulation is gradually increased without the assistance of flexible friction; when the friction of the flexible brush is increased, a certain brush trace is generated more severely when the friction is lower in current density (fig. 4b 1), the quality of the balance state is better when the current density is higher (fig. 4b 2), and finally the knots are difficult to remove after the current density is too large (fig. 4b 3-4 b 4). The mass is the best about 150A/dm 2 without friction, the mass is the best about 250A/dm 2 after friction is added, and the optimal current density is obviously improved, so that the flexible friction is obviously improved compared with the friction-free surface quality, and the coating leveling effect is obvious.
Hardness thickness analysis: the microhardness and thickness of each plating piece are measured by adopting an HXS-1000A digital intelligent microhardness meter and a Hitachi CMI730 handheld plating thickness meter, and the results are respectively shown in the left part and the right part of the figure 5, and compared with the conventional jet electrodeposition, the surface microhardness after dynamic flexible rotation friction assistance is higher, and can reach 546 HV when the current density is proper (about 250A/dm 2); the thickness is increased, and the thickness is reduced along with the increase of the current density due to certain mechanical removal, but the thickness is reduced after the friction is increased by more than 250A/dm 2 without friction, which indicates that the limit current density is increased after the friction is increased, and the utilization rate of the whole plating layer to the current is obviously improved, so that the surface hardness of the plating layer after the rotation friction assistance is obviously improved, the limit current density is increased, and the high-quality plating layer can be prepared more efficiently.
Tissue structure analysis: the microstructure of each coating was measured using a SmartLab kW X-ray diffractometer, the XRD pattern and grain size (calculated according to Scherrer's formula) results are shown in fig. 6, and the results at three current densities were examined, and it was seen that the microstructure of the coating was a face-centered cubic structure, and that the (111) crystal plane was always highly preferred, and neither was changed with current density (fig. 6 left). In addition, the grain sizes are all nano-scale, the trend of firstly decreasing and then increasing is presented, after the dynamic and flexible rotary friction assistance is added, the grain size refinement is remarkable, the average grain size is reduced, and the minimum reaches about 11.5 nm (right in fig. 6) particularly at the speed of 250A/dm 2; the flexible brush has the best hydrogen-expelling and impurity-removing effects under the current density, and the concentration polarization is serious and the friction auxiliary effect is reduced when the current density is too high.
As shown in the mechanism of figure 1, when the current density is controlled properly, the surface of the plating layer can be smooth and compact by only needing smaller flexible friction rotation speed, compared with the common jet electrodeposition, the plating layer has almost no defects of pinholes, pits, knots and the like, and after the dynamic flexible rotary friction assistance is introduced, the limiting current density and the current use efficiency are both improved, the optimal current density under friction is improved from 150A/dm 2 without friction to 250A/dm 2, the grain size is reduced to 11.5 nm, the microhardness is increased to 546 HV, and in conclusion, the jet electrodeposition after the dynamic flexible friction assistance is increased can efficiently prepare the high-quality nanocrystalline nickel plating layer.
The foregoing is merely a preferred embodiment of the invention, and it should be noted that modifications could be made by those skilled in the art without departing from the principles of the invention, which modifications would also be considered to be within the scope of the invention.
Claims (10)
1. The method for preparing the nanocrystalline nickel coating by dynamic flexible friction-assisted jet electrodeposition is characterized by comprising the following steps of:
providing a conductive workpiece cathode substrate; preparing an electroplating nickel solution;
A movable flexible rotary friction auxiliary device is additionally arranged on the jet electrodeposition device, enough nickel beads are added into an anode cavity, and a cathode substrate is clamped on a jet electrodeposition workbench;
Adding the nickel electroplating liquid into a jet flow deposition device, so that the nozzle reciprocates at a certain scanning speed and the brush rotates at a low speed to assist jet flow deposition work through flexible friction;
and cleaning and drying the cathode workpiece after the plating.
2. The method for preparing the nanocrystalline nickel coating by dynamic and flexible friction-assisted jet deposition according to claim 1, wherein the cathode substrate is firstly polished roughly by adopting metallographic sand paper before being cleaned, then polished finely by adopting a metallographic polisher, and then cleaned and dried by adopting deionized water, alcohol and acetone.
3. The method for preparing the nanocrystalline nickel coating by dynamic flexible friction-assisted jet deposition according to claim 1 or 2, wherein the cathode substrate is made of metal or graphite.
4. The method for preparing a nanocrystalline nickel coating by dynamic flexible friction-assisted jet deposition according to claim 1, wherein the step of preparing an electroplating nickel solution comprises the steps of: heating deionized water to 80-100 ℃, adding boric acid, and then sequentially adding nickel sulfate hexahydrate and nickel chloride hexahydrate as nickel element sources; the addition amount of boric acid is 20-60 g/L, the addition amount of nickel sulfate hexahydrate is 240-280 g/L, and the addition amount of nickel chloride hexahydrate is 20-60 g/L.
5. The method for preparing the nanocrystalline nickel coating by dynamic and flexible friction-assisted jet deposition according to claim 1 or 4, wherein hydrochloric acid is added to maintain the pH of the solution at 3.8-4.2 after preparing the nickel electroplating solution.
6. The method for preparing the nanocrystalline nickel plating by dynamic flexible friction-assisted jet deposition according to claim 1 or 4, wherein the flexible brush material adopted by the dynamic flexible rotary friction-assisted device is bristle, and the diameter of the nickel beads is within 5-10 mm.
7. The method for preparing a nanocrystalline nickel coating by dynamic flexible friction-assisted jet electrodeposition according to claim 1, wherein the jet electrodeposition parameters are: the temperature of the electroplating solution is 35-55 ℃, the current density is 150-350A/dm 2, the scanning speed is 300-1200 mm/min, the deposition time is 40-80 min, the nozzle flow is 200-300L/h, the rotating friction rotating speed is 0-8 r/min, and the interelectrode gap is 1-2 mm.
8. An apparatus for preparing a nanocrystalline nickel coating by dynamic flexible friction-assisted jet deposition used in the method according to any one of claims 1 to 7, characterized in that the apparatus comprises: the device comprises a frame mechanism, an X-axis transmission mechanism, a Z-axis transmission mechanism, a rotary friction mechanism and a plating solution circulation mechanism; the X-axis transmission mechanism is arranged on the frame mechanism and used for controlling the reciprocating and cyclic scanning movement of the jet electrodeposition nozzle, the Z-axis transmission mechanism controls the interelectrode gap, the rotary friction mechanism enables the brush to flexibly rotate and rub the surface of the cathode to improve the jet electrodeposition quality, and the plating solution circulation mechanism circulates and sprays the plating solution of jet electrodeposition.
9. The apparatus for preparing a nanocrystalline nickel coating by kinetic flexible friction-assisted jet deposition according to claim 8, wherein the rotary friction mechanism comprises: the device comprises a motor, a driving wheel, a driven wheel, a nozzle, a brush wheel, a driven wheel, a fixed bearing, an anode connecting piece and an anode cavity; the plating solution circulating mechanism comprises an anode cavity, a fixed bearing is arranged on the anode cavity, the anode cavity is fixed through an anode connecting piece, a nozzle is arranged at the bottom of the anode cavity, a cathode workpiece is positioned below the nozzle, the anode cavity penetrates through the fixed bearing, a driven wheel is arranged on the outer ring of the fixed bearing, a brush wheel is arranged below the driven wheel, a motor is arranged on the side edge of the anode connecting piece, a driving wheel is arranged on the motor, the driving wheel is connected with the driven wheel through a synchronous belt, and the top end of the anode cavity is connected with the plating solution circulating mechanism through a pipeline.
10. The apparatus for preparing a nano-crystalline nickel coating by dynamic and flexible friction-assisted jet deposition according to claim 9, wherein the anode connecting piece is integrally installed on a sliding table of the Z-axis transmission mechanism.
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| CN202410421595.1A CN118292063A (en) | 2024-04-09 | 2024-04-09 | Device and method for preparing nanocrystalline nickel coating by dynamic flexible friction-assisted jet flow electrodeposition |
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| CN202410421595.1A CN118292063A (en) | 2024-04-09 | 2024-04-09 | Device and method for preparing nanocrystalline nickel coating by dynamic flexible friction-assisted jet flow electrodeposition |
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