CN111118582B - Preparation device and method of Ni-SiC composite coating with (220) high preferred orientation - Google Patents
Preparation device and method of Ni-SiC composite coating with (220) high preferred orientation Download PDFInfo
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- CN111118582B CN111118582B CN202010024213.3A CN202010024213A CN111118582B CN 111118582 B CN111118582 B CN 111118582B CN 202010024213 A CN202010024213 A CN 202010024213A CN 111118582 B CN111118582 B CN 111118582B
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- 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
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D17/00—Constructional parts, or assemblies thereof, of cells for electrolytic coating
- C25D17/10—Electrodes, e.g. composition, counter electrode
- C25D17/12—Shape or form
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D21/00—Processes for servicing or operating cells for electrolytic coating
- C25D21/06—Filtering particles other than ions
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- 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
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- 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
- C25D5/08—Electroplating with moving electrolyte e.g. jet electroplating
Abstract
The invention discloses a preparation method of a Ni-SiC composite coating with (220) high preferred orientation, which comprises the following steps: connecting a titanium rod (14) with the positive electrode of a direct current power supply (1), connecting a steel plate (5) with the negative electrode of the direct current power supply (1), enabling a plating solution to flow from a liquid inlet (3) at a flow rate of 120-2. The titanium rod (14) is not consumed in the reaction process due to the stable chemical property, and a stable electric field environment is formed between the lower end of the titanium rod (14) and the upper surface of the steel plate (5). Under the environment, the reduced nickel atoms and SiC particles quickly form a Ni-SiC composite coating with (220) high preferred orientation to be deposited on the steel plate (5). Compared with the conventional oriented Ni-SiC composite coating, the Ni-SiC composite coating with the structure has the advantages of smooth surface and strong bonding force.
Description
Technical Field
The invention belongs to the field of electrochemical deposition of special processing, and particularly relates to a device and a method for preparing a Ni-SiC composite coating with (220) high preferred orientation.
Background
The preparation method of the nickel coating which is commonly used at home and abroad at present mainly adopts the traditional electrodeposition, the working principle is that a workpiece is taken as a cathode, a nickel plate is taken as an anode, the whole body is immersed in a plating solution, and nickel metal ions in the plating solution are reduced to form the coating on the surface of the workpiece to be plated. However, the traditional electroplating method has the defects of insufficient stirring speed, low ion transmission speed and uneven ion distribution in the plating solution, so that concentration polarization phenomenon occurs. When the deposition current density is high, the concentration polarization phenomenon is more serious, and the surface quality of the obtained coating is poor. In addition, the coating prepared by the traditional electroplating method usually has the defects of pinholes, pockmarks and the like. Therefore, the deposition efficiency is low, and the poor quality of the coating is a disadvantage of the traditional electroplating method.
The spray electrodeposition technology is a deposition mode derived on the basis of the traditional electrodeposition, the deposition principle of the spray electrodeposition technology is not different from that of the common electrodeposition, but the spray electrodeposition technology adopts the steps that electroplating solution is sprayed onto the surface of a cathode at a certain speed and pressure, a loop is formed between the cathode and an anode through the electroplating solution, and at the moment, the spraying flow area generates electrodeposition due to the passing of current. The deposition in the mode has special flow field and electric field, the high-speed flowing liquid flow accelerates the transmission speed of ions in the deposition process, strong disturbance enables the ions to be distributed more uniformly, concentration polarization is reduced, and meanwhile deposition of impurities can be reduced, so that a coating with good quality can be obtained. Because the jet electrodeposition has the characteristic of selective deposition, and the jet flow field limits the strength and distribution of an electric field, a plurality of coating forms which cannot be obtained by the traditional electrodeposition can be obtained by controlling the flow field and electric parameters.
During electrodeposition, a preferred orientation (texture) of crystal planes often occurs, i.e., in the deposited layer, a considerable number of crystal grains exhibit a certain co-orientation characteristic, and if the orientation of the crystal grains is highly concentrated in a certain orientation, the preferred orientation is called highAnd (3) direction. In recent years, the research on the preferred orientation of crystal grains in the nickel-based metal coating prepared by electrodeposition has also received much attention. When researchers prepare the Ni-SiC composite coating by using an electrodeposition method, the research finds that the grain orientation of the coating gradually evolves from (200) to (111) along with the increase of the SiC content, and the corrosion resistance of the coating is improved when the coating structure is in the preferred orientation of (111). There are researchers in preparing Ni-Cu/Al2O3When the plating was carried out in combination, it was found that Al contained in the plating solution was accompanied by2O3The content of the nano particles is increased, the coating gradually evolves to a (111) preferred orientation structure, and the hardness, the wear resistance and the corrosion resistance of the coating are improved. In the preparation of the Ni/diamond composite coating by using the traditional electrodeposition method, researchers find that the addition of the additive BEO can cause the coating to generate (200) preferred orientation, and the wear resistance of the coating is improved.
However, the research on the crystal orientation of the nickel-based composite coating is mainly focused on the (111) and (200) orientations, and the research on the (220) high-preferential orientation of the Ni-SiC composite coating is not reported. The Ni-SiC composite coating with (220) high preferred orientation is difficult to be efficiently prepared by the prior art and the method.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art and provides a device and a method for preparing a Ni-SiC composite coating with (220) high preferred orientation.
The technical scheme of the invention is as follows:
a preparation device of a Ni-SiC composite coating with (220) high preferred orientation is disclosed, a titanium rod (14) is connected with the positive electrode of a direct current power supply (1) through an anode lead (13), a steel plate (5) is fixed on a cathode support plate (6), the steel plate (5) is connected with the negative electrode of the direct current power supply (1) through a cathode lead (2), a liquid inlet (3) is connected with an anode cylinder (11), the upper end of the anode cylinder (11) is connected with a rubber plug (12), the lower end of the anode cylinder (11) is connected with a nozzle (8), a nickel bead (10) is placed inside the anode cylinder (11), a filter screen (9) is placed between the nickel bead (10) and the nozzle (8), the titanium rod (14) penetrates through the rubber plug (12), the nickel bead (10) and the filter screen (9) in turn and is placed inside the anode cylinder (11), a plating solution flows in from the liquid inlet (3) and is sprayed out to the upper surface of the steel plate (5) from the nozzle (8), finally flows out from a liquid outlet (7) of the cathode deposition tank (4).
The preparation device of the Ni-SiC composite coating with (220) high preferred orientation is characterized in that the liquid inlet (3), the cathode deposition groove (4), the cathode supporting plate (6), the nozzle (8), the filter screen (9) and the anode cylinder (11) are made of PLA materials, the rubber plug (12) is made of rubber materials, and the materials are all not conductive.
According to the preparation device of the Ni-SiC composite coating with the (220) high preferred orientation, the titanium rod (14) is used as a transmission electrode and connected with the positive electrode of the direct current power supply (1), current is conducted to the nickel beads (10) which are in close contact with the titanium rod, so that the nickel beads (10) become the positive electrode, the nickel beads (10) are consumed in the reaction process to supplement nickel ions in the plating solution, and the titanium rod (14) is not consumed in the reaction process due to the stable chemical property of the titanium rod, so that a stable electric field environment is formed between the lower end of the titanium rod (14) and the upper surface of the steel plate (5), and the reaction process is more stable.
According to the preparation device of the Ni-SiC composite coating with the (220) high preferred orientation, the nozzle (8) adopts a shrinkage hole structure, and the plating solution is bundled into a liquid column with the diameter of 5mm to be sprayed onto the upper surface of the steel plate (5).
According to the preparation device of the Ni-SiC composite coating with the (220) high preferred orientation, the filter screen (9) is used for filtering the plating solution, and particles falling off when the nickel beads (10) are consumed are prevented from being sprayed out along with the plating solution, so that the quality of the coating is prevented from being influenced.
The preparation device of the Ni-SiC composite coating with the (220) high preferred orientation comprises the following components: 300g/l of nickel sulfate, 40g/l of nickel chloride, 40g/l of boric acid, 3g/l of SiC nanoparticles, 1g/l of saccharin and 0.5g/l of OP-10 are dissolved uniformly by heating and stirring.
A preparation method of a Ni-SiC composite coating with (220) high preferred orientation comprises the following steps:
step 1: adjusting the distance between the lower end of the titanium rod (14) and the nozzle (8) to be 5mm, and the distance between the nozzle (8) and the upper surface of the steel plate (5) to be 3 mm;
step 2: the plating solution is adjusted to flow in from the liquid inlet (3) at a flow rate of 150L/h, and the reaction process is kept constant;
and step 3: starting the direct current adjustable power supply (1), and adjusting the current density to 220A/dm2And nickel metal ions and SiC nano particles in the plating solution rapidly form a Ni-SiC composite plating layer to be deposited on the cathode steel plate (5).
According to the device and the method for preparing the Ni-SiC composite coating with the (220) high preferred orientation, the prepared Ni-SiC composite coating is of a (220) high preferred orientation structure, and the (220) preferred orientation coefficient is more than 95%.
Compared with the prior art, the invention has the following beneficial effects:
1. the nozzle is designed to adopt a shrinkage hole structure, plating solution can be converged into a bundle of liquid column to be sprayed out to the surface of the steel plate at a high speed, the common plating solution concentration polarization phenomenon in the traditional electroplating is effectively improved due to the high-speed flowing of the plating solution, the upper limit of the deposition current density is improved, and the preparation speed of the plating layer is improved.
2. The titanium rod is used as a transmission electrode to conduct current to the nickel ball which is in contact with the titanium rod, the nickel ball is consumed to supplement the nickel ions reduced in the plating solution, and the titanium rod is not consumed due to the stable chemical property of the titanium rod, so that stable electric field distribution can be formed between the titanium rod and the steel plate, and the deposition process is more stable.
3. The prepared Ni-SiC composite coating with (220) high preferred orientation has the (220) preferred orientation coefficient as high as 97.1 percent (shown in figure 2).
4. Compared with the Ni-SiC composite coating with the conventional orientation, the prepared Ni-SiC composite coating with (220) high preferred orientation has the advantages of flat and smooth surface appearance, no obvious defects such as pinholes, pockmarks and the like (as shown in figure 3).
5. The prepared Ni-SiC composite coating with (220) high preferred orientation has about 2 times higher coating bonding force compared with the Ni-SiC composite coating with the conventional orientation (as shown in figure 4).
Drawings
FIG. 1 is a schematic view of an apparatus for preparing a Ni-SiC composite coating having a (220) high preferred orientation;
FIG. 2 is an XRD inspection of a Ni-SiC composite coating having a (220) high preferred orientation and a conventionally oriented Ni-SiC composite coating;
FIG. 3 is a surface topography inspection map of a Ni-SiC composite coating having a (220) high preferred orientation and a conventionally oriented Ni-SiC composite coating;
FIG. 4 is a scratch topography inspection chart of a Ni-SiC composite coating with a (220) high preferred orientation and a Ni-SiC composite coating with a conventional orientation.
In the figure: 1. the device comprises a direct current power supply, 2, a cathode wiring, 3, a liquid inlet, 4, a cathode deposition tank, 5, a steel plate, 6, a cathode supporting plate, 7, a liquid outlet, 8, a nozzle, 9, a filter screen, 10, nickel beads, 11, an anode cylinder, 12, a rubber plug, 13, an anode wiring, 14 and a titanium rod.
Detailed Description
The present invention will be described in detail with reference to specific examples.
Referring to fig. 1, a device for preparing a Ni-SiC composite coating having a (220) high preferred orientation comprises a dc power supply 1, a cathode connection 2, a liquid inlet 3, a cathode deposition tank 4, a steel plate 5, a cathode support plate 6, a liquid outlet 7, a nozzle 8, a filter screen 8, nickel beads 10, an anode cylinder 11, a rubber plug 12, an anode connection 13 and a titanium rod 14. Titanium bar 14 is connected with 1 anodal with DC power supply through positive pole wire 13, steel sheet 5 is fixed on negative pole backup pad 6, steel sheet 5 is connected with 1 negative pole of DC power supply through negative pole wire 2, inlet 3 links to each other with positive pole jar 11, 11 upper ends of positive pole jar link to each other with plug 12, 11 lower extremes of positive pole jar link to each other with nozzle 8, nickel pearl 10 is placed inside positive pole jar 11, filter screen 9 is placed between nickel pearl 10 and nozzle 8, titanium bar 14 runs through plug 12 according to this, nickel pearl 10 and filter screen 9, place in inside positive pole jar 11, the plating solution flows in from inlet 3, spout to steel sheet 5 upper surface from nozzle 8, flow out from the liquid outlet 7 of negative pole sedimentation tank 4 at last. The nozzle 8 adopts a shrinkage hole structure, and sprays the plating solution beam into a liquid column with the diameter of 5mm to the upper surface of the steel plate 5. The filter screen 9 is used for filtering the plating solution and preventing the falling particles from being sprayed out along with the plating solution when the nickel beads 10 are consumed, thereby influencing the quality of the plating layer. The plating solution comprises the following components: 300g/l of nickel sulfate, 40g/l of nickel chloride, 40g/l of boric acid, 3g/l of SiC nanoparticles, 1g/l of saccharin and 0.5g/l of OP-10 are dissolved uniformly by heating and stirring.
The invention provides a preparation method of a Ni-SiC composite coating with (220) high preferred orientation, which comprises the following steps:
step 1: adjusting the distance between the lower end of the titanium rod 14 and the nozzle 8 to be 5mm, and the distance between the nozzle 8 and the upper surface of the steel plate 5 to be 3 mm;
step 2: adjusting the plating solution to flow in from the liquid inlet 3 at a flow rate of 150L/h, and keeping the solution constant in the reaction process;
and step 3: starting the direct current adjustable power supply 1, and adjusting the current density to 220A/dm2The nickel metal ions and the SiC nano-particles in the plating solution rapidly form a Ni-SiC composite plating layer to be deposited on the cathode steel plate 5. The prepared Ni-SiC composite plating layer is of a (220) high preferred orientation structure, and the (220) preferred orientation coefficient is more than 95%.
FIG. 2 is an XRD detection diagram of the Ni-SiC composite coating, and the Ni-SiC composite coating prepared by the method has obvious (220) high preferred orientation, and the (220) preferred orientation coefficient reaches 97.1%.
FIG. 3 is a surface topography inspection chart of a Ni-SiC composite plating layer with (220) high preferred orientation and a Ni-SiC composite plating layer with a conventional orientation, wherein the Ni-SiC composite plating layer with the conventional orientation has rough surface and has defects of pinholes, pits and the like, while the Ni-SiC composite plating layer with (220) high preferred orientation has smooth and flat surface and no defects of pinholes, pits and the like.
FIG. 4 is a scratch morphology detection graph of a Ni-SiC composite plating layer with (220) high preferred orientation and a Ni-SiC composite plating layer with a conventional orientation, wherein the bonding force of the Ni-SiC composite plating layer with the conventional orientation is 20.5N, and the bonding force of the Ni-SiC composite plating layer with (220) high preferred orientation reaches 61.6N, which is improved by about two times.
It will be understood that modifications and variations can be made by persons skilled in the art in light of the above teachings and all such modifications and variations are intended to be included within the scope of the invention as defined in the appended claims.
Claims (7)
1. A preparation method of a Ni-SiC composite coating with (220) high preferred orientation is characterized in that a titanium rod (14) is connected with the positive pole of a direct current power supply (1) through an anode lead (13), a steel plate (5) is fixed on a cathode support plate (6), the steel plate (5) is connected with the negative pole of the direct current power supply (1) through a cathode lead (2), and a liquid inlet (3) and an anode are connectedThe device comprises a cylinder (11), an anode cylinder (11), a rubber plug (12), a nozzle (8), a nickel bead (10), a filter screen (9), a titanium rod (14), a liquid inlet (3), a steel plate (5), and a liquid outlet (7) of a cathode deposition tank (4), wherein the upper end of the anode cylinder (11) is connected with the rubber plug (12), the lower end of the anode cylinder (11) is connected with the nozzle (8), the nickel bead (10) is arranged inside the anode cylinder (11), the filter screen (9) is arranged between the nickel bead (10) and the nozzle (8), the titanium rod penetrates through the rubber plug (12), the nickel bead (10) and the filter screen (9) and is arranged inside the anode cylinder (11) in sequence, and plating liquid flows in from the liquid inlet (3), is sprayed out of the nozzle (8) to the upper surface of the steel plate (5), and finally flows out of the liquid outlet (7) of the cathode deposition tank (4); when in use, the distance between the lower end of the titanium rod (14) and the nozzle (8) is adjusted to be 5mm, and the distance between the nozzle (8) and the upper surface of the steel plate (5) is adjusted to be 3 mm; the plating solution is adjusted to flow in from the liquid inlet (3) at a flow rate of 150L/h, and the reaction process is kept constant; starting the direct current power supply (1), and adjusting the current density to 220A/dm2And nickel metal ions and SiC nano particles in the plating solution quickly form a Ni-SiC composite plating layer to be deposited on the steel plate (5).
2. The method for preparing the Ni-SiC composite coating with (220) high preferred orientation according to claim 1, wherein the liquid inlet (3), the cathode deposition tank (4), the cathode support plate (6), the nozzle (8), the filter screen (9) and the anode cylinder (11) are PLA materials, the rubber plug (12) is rubber material, and the above materials are all not conductive.
3. The method for preparing the Ni-SiC composite coating with (220) high preferred orientation according to claim 1, wherein the titanium rod (14) is used as a transmission electrode and is connected with the positive electrode of the direct current power supply (1), current is conducted to the nickel beads (10) which are in close contact with the titanium rod, so that the nickel beads (10) become anodes, the nickel beads (10) are consumed in the reaction process to supplement nickel ions in the coating solution, and the titanium rod (14) is not consumed in the reaction process due to the stable chemical property of the titanium rod, so that a stable electric field environment is formed between the lower end of the titanium rod (14) and the upper surface of the steel plate (5), and the reaction process is more stable.
4. The method for preparing a Ni-SiC composite coating having a (220) high preferred orientation according to claim 1, characterized in that the spray nozzles (8) spray the coating solution onto the upper surface of the steel sheet (5) in a liquid column having a diameter of 5mm using a constricted hole structure.
5. The method for preparing a Ni-SiC composite coating having a (220) high preferred orientation according to claim 1, wherein a strainer (9) is used to filter the plating solution to prevent particles dropped off when the nickel beads (10) are consumed from being ejected with the plating solution to affect the coating quality.
6. The method for preparing a Ni-SiC composite coating having a (220) high preferred orientation according to claim 1, characterized in that the bath composition is: 300g/l of nickel sulfate, 40g/l of nickel chloride, 40g/l of boric acid, 3g/l of SiC nanoparticles, 1g/l of saccharin and 0.5g/l of OP-10 are dissolved uniformly by heating and stirring.
7. The method for preparing the Ni-SiC composite coating with (220) high preferred orientation according to any one of claims 1 to 6, wherein the prepared Ni-SiC composite coating is of a (220) high preferred orientation structure, and the (220) preferred orientation coefficient is more than 95%.
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2020
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