CN114990671A - Electroplating method for improving corrosion resistance of water pump pull rod - Google Patents

Electroplating method for improving corrosion resistance of water pump pull rod Download PDF

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CN114990671A
CN114990671A CN202210715778.5A CN202210715778A CN114990671A CN 114990671 A CN114990671 A CN 114990671A CN 202210715778 A CN202210715778 A CN 202210715778A CN 114990671 A CN114990671 A CN 114990671A
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sodium
pull rod
corrosion resistance
solution
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CN114990671B (en
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吴玉林
梅益涛
梅剑峰
程志强
王维龙
何建军
钟国晟
凤琦
张逍
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Anhui Wolong Pump & Valve Co ltd
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    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D13/00Electrophoretic coating characterised by the process
    • C25D13/22Servicing or operating apparatus or multistep processes
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/02Cleaning or pickling metallic material with solutions or molten salts with acid solutions
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    • C23G1/086Iron or steel solutions containing HF
    • CCHEMISTRY; METALLURGY
    • C23COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/14Cleaning or pickling metallic material with solutions or molten salts with alkaline solutions
    • C23G1/19Iron or steel
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D13/00Electrophoretic coating characterised by the process
    • C25D13/02Electrophoretic coating characterised by the process with inorganic material
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Abstract

The invention relates to an electrodeposition method, in particular to an electroplating method for improving the corrosion resistance of a water pump pull rod, which comprises the following steps: the cubic boron nitride and the alumina are used as the high-hardness nano particles to be dispersed in the matrix metal, so that the hardness of the coating is improved, the corrosion medium and the matrix metal can be effectively separated, the area of the matrix metal exposed in the corrosion solution is reduced, and the further corrosion of the corrosion solution to the coating is prevented. Meanwhile, the added Na and P elements can play a synergistic role with the nano particles, so that the microstructure of the coating is obviously improved, the binding force between the substrate metal and the ceramic base layer is favorably enhanced, and the corrosion resistance of the material is further improved. The acid washing activation time of the base material is prolonged, the binding force with the coating is improved by manufacturing the rough base surface, the effects of phase change and brittle fracture of the coating and the base material caused by the difference of expansion coefficients are weakened, and the process plays an important role in corrosion prevention of the water pump pull rod.

Description

Electroplating method for improving corrosion resistance of water pump pull rod
Technical Field
The invention belongs to the field of material surface modification, in particular relates to a corrosion-resistant electroplating method for improving pump parts, and particularly relates to an electroplating method for improving corrosion resistance of a water pump pull rod.
Background
With the rapid development of modern science and technology, the requirements of the industrial field on the surface performance of materials are continuously improved, and surface engineering becomes an important branch of material science. The surface of the material is coated or modified to change the form, chemical composition and tissue structure of the solid surface, so that the performance of the local or whole surface of the material can be improved, and the surface is endowed with new functions in the aspects of mechanics, optics, electromagnetism, heat, physical chemistry and the like. In the research of material surface modification and strengthening treatment, coatings and plating layers with specific functions show irreplaceable important roles. At present, there are various methods for forming coatings and coatings, such as: thermal spraying, chemical vapor deposition, physical vapor deposition, self-propagating high temperature synthesis, and electrochemical deposition-based electroplating techniques, among others; among them, the composite plating technology developed on the basis of the electroplating technology has attracted much attention in the field of material surface modification.
The composite coating is a special coating formed by uniformly mixing one or more insoluble solid particles, inert particles, fibers and the like into a metal deposition layer by a metal deposition method. The basic components of the composite coating are two types, one type is metal forming the coating through reduction reaction, and the metal can be called as matrix metal, and the matrix metal is a uniform continuous phase; the other is insoluble particles, which are usually discontinuously dispersed in the matrix metal. The phase interface between the matrix metal and the insoluble particles in the composite coating is basically clear, mutual diffusion hardly occurs, but the composite coating has the comprehensive performance of the matrix metal and the insoluble particles. The preparation process of the composite coating is simple, the cost is low, the composite coating can be operated at normal temperature, the internal properties of the main material are not influenced, and the composite coating is one of effective ways for improving the surface performance of the material. Research on composite coatings has been done for half a century, but practical industrial application of composite coatings has been almost two to thirty years. The main reason for this is that the composite coating is mostly carried with micron-sized particles with large particle size, and the prepared composite coating has rough surface and poor corrosion resistance, and these defects largely limit the further development and application of the composite coating. Therefore, developing an electroplating technology with a smooth surface and modified nano particles dispersed and uniformly distributed in the coating is of great significance for improving the corrosion resistance and wear resistance of the material.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention aims to provide an electroplating method for improving the corrosion resistance of a water pump pull rod, so as to solve the problems in the technical background.
In order to achieve the above purpose, the invention is realized by the following technical method:
s1, weighing a certain amount of medicine, and adding the medicine into deionized water to dissolve the medicine to prepare the main electroplating solution, wherein the specific concentration is as follows: the concentration of nickel chloride is 140-260g/L, the concentration of boric acid is 33-46g/L, the concentration of sodium hypophosphite is 23-48g/L, and the concentration of sodium citrate is 0.35-0.96 g/L;
s2, weighing a certain amount of 8-16g of aluminum isopropoxide solid by using an electronic balance, putting the weighed aluminum isopropoxide solid in a grinding dish to grind the aluminum isopropoxide into powder, putting 250mL of deionized water on a constant-temperature magnetic stirrer platform to heat, wherein the water temperature isAdding refined isopropanol aluminum powder at a certain rotation speed when the temperature reaches 85 ℃, stirring, dripping a certain amount of nitric acid into the solution while stirring, continuously stirring for a period of time, adjusting the temperature of a water bath kettle to 50-90 ℃, standing for 5-15h at a constant temperature, and obtaining Al with good stability and high transparency 2 O 3 Sol;
s3, placing a certain amount of deionized water into a colorimetric tube, adding a proper amount of non-ionic surfactant sodium dodecyl sulfate with the concentration of 0.05-0.15g/L, carrying out ultrasonic oscillation to uniformly disperse the deionized water, weighing a certain amount of cubic boron nitride with the concentration of 5-25g/L, adding the weighed cubic boron nitride into the deionized water, alternately carrying out eddy current uniform mixing and ultrasonic oscillation for several times until powdery cubic boron nitride cannot be seen in a suspended emulsion in the colorimetric tube, weighing a certain amount of dispersed suspended emulsion, placing the weighed suspended emulsion into a small beaker, dropwise adding a small amount of electroplating main solution under the action of mechanical stirring, and stirring uniformly;
s4, placing the electroplating solution prepared in the step S1 on a magnetic stirrer, and gradually and slowly adding the Al prepared in the steps S2 and S3 according to a certain volume ratio under the action of mechanical stirring 2 O 3 Sol and cubic boron nitride suspension;
s5, polishing the small steel sheet by using sand paper to remove a surface oxidation film, and then carrying out chemical degreasing and acid washing activation, wherein the chemical degreasing solution mainly comprises the following components in percentage by weight: 35-96g/L of sodium hydroxide, 12-65g/L of sodium carbonate, 35-67g/L of sodium phosphate and 2.5-9.6g/L of sodium silicate, wherein the acid-washing solution mainly comprises the following components in percentage by weight: 18-46mL/L hydrochloric acid with the concentration of 1.05g/mL and 36-78 mL/L35% hydrofluoric acid, and the specific implementation steps comprise placing a small steel sheet in the solution, and carrying out ultrasonic treatment for a period of time;
and S6, wiping the pretreated matrix, and placing the matrix in a self-made electrophoresis tank. The nickel sheet is used as an anode, the stainless steel sheet is used as a cathode, the electrophoretic deposition is carried out under the magnetic stirring by adopting a structure of double anodes and single cathode, and the current density is set to be 3-8A/dm 2 The deposition time is 160-380S;
s7, putting the electroplated material into an SX4-10 box type resistance furnace, heating to a specific temperature according to a certain heating rate, and preserving the temperature for a period of time to obtain the prepared material.
Preferably, the rotation speed of the constant-temperature magnetic stirrer in the step S2 is set to be 300r/min, and the stirring time is 3 h.
Preferably, the amount of nitric acid added in step S2 is 0.625 mL.
Preferably, Al in step S4 2 O 3 The volume ratio of the sol to the cubic boron nitride suspension to the electroplating main solution is 2: 0.8: 97.2.
preferably, the chemical degreasing time period in step S5 is 23 min.
Preferably, in step S7, the temperature rising speed is 10 ℃/min, the heat preservation temperature is 500 ℃, and the heat preservation time is 7 min.
Compared with the prior art, the invention has the following beneficial effects: in conclusion, the invention discloses an electroplating process, which utilizes cubic boron nitride and aluminum oxide as high-hardness nano particles to be dispersed in matrix metal, so that the hardness of a coating is improved, a corrosive medium and the matrix metal can be effectively separated, the area of the matrix metal exposed in a corrosive solution is reduced, and the further corrosion of the coating by the corrosive solution is prevented. Meanwhile, the added Na and P elements can play a synergistic effect with the nano particles, so that the microstructure of the coating is obviously improved, the bonding force between the substrate metal and the ceramic base layer is enhanced, and the corrosion resistance of the material is further improved. In addition, the acid washing activation time of the base material is prolonged, the binding force with the coating is improved by manufacturing a rough base surface, the effects of phase change and brittle fracture of the coating and the base material caused by the difference of expansion coefficients are weakened, and the process plays an important role in corrosion prevention of the water pump pull rod.
Drawings
FIG. 1 is a graph of the wear resistance of coatings prepared according to example 1 of the present invention and comparative examples 1-3.
FIG. 2 is a scan of the preparation of example 2 of the present invention and comparative examples 3-5.
FIG. 3 is a polarization graph of examples 1 to 3 and comparative examples 7 to 8.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides an electroplating process for improving corrosion resistance of a water pump pull rod, which comprises the following specific steps:
s1, weighing a certain amount of medicine, and adding the medicine into deionized water to dissolve the medicine to prepare the main electroplating solution, wherein the specific concentration is as follows: 140-260g/L of nickel chloride, 33-46g/L of boric acid, 23-48g/L of sodium hypophosphite and 0.35-0.96g/L of sodium citrate;
s2, weighing a certain amount of 8-16g aluminum isopropoxide solid by using an electronic balance, putting the weighed aluminum isopropoxide solid in a grinding dish to grind aluminum isopropoxide into powder, putting 250mL deionized water on a constant-temperature magnetic stirrer platform to heat, adding the refined aluminum isopropoxide powder to stir at a certain rotating speed when the water temperature reaches 85 ℃, dripping a certain amount of nitric acid into the solution while stirring, continuing to stir for a period of time, adjusting the temperature of a water bath kettle to 50-90 ℃ after stirring, standing at the constant temperature for 5-15h, and obtaining Al with good stability and high transparency 2 O 3 Sol;
s3, placing a certain amount of deionized water into a colorimetric tube, adding a proper amount of nonionic surfactant sodium dodecyl sulfate with the concentration of 0.05-0.15g/L, carrying out ultrasonic oscillation to uniformly disperse the deionized water, weighing a certain amount of cubic boron nitride with the concentration of 5-25g/L, adding the weighed cubic boron nitride into the deionized water, alternately carrying out eddy current uniform mixing and ultrasonic oscillation for several times until powdery cubic boron nitride cannot be seen in the suspended emulsion in the colorimetric tube, weighing the fixed amount of dispersed suspended emulsion, placing the suspended emulsion in a small beaker, dropwise adding a small amount of electroplating main solution under the action of mechanical stirring, and stirring uniformly;
s4, placing the electroplating solution prepared in the step S1 on a magnetic stirrer, and gradually and slowly adding the Al prepared in the steps S2 and S3 according to a certain volume ratio under the action of mechanical stirring 2 O 3 Sol and cubic boron nitride suspension;
s5, polishing the small steel sheet by using sand paper to remove a surface oxidation film, and then carrying out chemical degreasing and acid washing activation, wherein the chemical degreasing solution mainly comprises the following components in percentage by weight: 35-96g/L of sodium hydroxide, 12-65g/L of sodium carbonate, 35-67g/L of sodium phosphate and 2.5-9.6g/L of sodium silicate, wherein the formula of the acid-washing solution mainly comprises the following components: 18-46mL/L hydrochloric acid with the concentration of 1.05g/mL and 36-78 mL/L35% hydrofluoric acid, and the specific implementation steps comprise placing a small steel sheet in the solution, and carrying out ultrasonic treatment for a period of time;
and S6, wiping the pretreated matrix, and placing the matrix in a self-made electrophoresis tank. The nickel sheet is used as an anode, the stainless steel sheet is used as a cathode, the electrophoretic deposition is carried out under the magnetic stirring by adopting a structure of double anodes and single cathode, and the current density is set to be 3-8A/dm 2 The deposition time is 160-380S;
s7, putting the electroplated material into an SX4-10 box type resistance furnace, heating to a specific temperature according to a certain heating rate, and preserving the temperature for a period of time to obtain the prepared material.
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention. It should be noted that the features in the following embodiments and examples may be combined with each other without conflict.
Example 1
S1, weighing a certain amount of medicine, and adding the medicine into deionized water to dissolve the medicine to prepare the main electroplating solution, wherein the specific concentration is as follows: the concentration of nickel chloride is 180g/L, and the concentration of boric acid is 38 g/L;
s2, weighing a certain amount of 9.6g of aluminum isopropoxide solid by using an electronic balance, putting the weighed aluminum isopropoxide solid in a grinding dish to grind aluminum isopropoxide into powder, putting 250mL of deionized water on a constant-temperature magnetic stirrer platform to heat, and adding the refined aluminum isopropoxide when the water temperature reaches 85 DEG CStirring aluminum alkoxide powder at a certain rotation speed of 300r/min for 3h, dripping 0.625mL of nitric acid into the solution while stirring, continuously stirring for a period of time, adjusting the temperature of a water bath kettle to 75 ℃, standing for 8h at a constant temperature after stirring is finished, and thus obtaining Al with good stability and high transparency 2 O 3 Sol;
s3, placing a certain amount of deionized water into a colorimetric tube, adding a proper amount of non-ionic surfactant sodium dodecyl sulfate with the concentration of 0.085g/L, carrying out ultrasonic oscillation to uniformly disperse the deionized water, weighing a certain amount of cubic boron nitride with the concentration of 3.5g/L, adding the weighed cubic boron nitride into the deionized water, alternately carrying out eddy current uniform mixing and ultrasonic oscillation for a plurality of times until powdery cubic boron nitride cannot be seen in a suspended emulsion in the colorimetric tube, measuring the quantitatively dispersed suspended emulsion, placing the measured suspended emulsion into a small beaker, dropwise adding a small amount of electroplating main solution under the mechanical stirring action, and stirring uniformly;
s4, placing the electroplating solution prepared in the step S1 on a magnetic stirrer, and stirring the electroplating solution according to the proportion of 2: 0.8: 97.2 by volume was gradually and slowly added to the Al prepared in steps S2 and S3 2 O 3 Sol and cubic boron nitride suspension;
s5, polishing the small steel sheet by using sand paper to remove a surface oxidation film, and then carrying out chemical degreasing and acid washing activation, wherein the chemical degreasing solution mainly comprises the following components: 58g/L of sodium hydroxide, 32g/L of sodium carbonate, 47g/L of sodium phosphate and 6.9g/L of sodium silicate, wherein the acid-washing solution mainly comprises the following components in percentage by weight: 26mL/L hydrochloric acid with the concentration of 1.05g/mL and 54 mL/L35% hydrofluoric acid, and the specific implementation steps comprise placing the small steel sheet in the solution, and carrying out ultrasonic treatment for a period of time, wherein the chemical oil removal time is 23min, and the acid cleaning activation time is 270 s;
and S6, wiping the pretreated matrix, and placing the matrix in a self-made electrophoresis tank. The nickel sheet is used as an anode, the stainless steel sheet is used as a cathode, the electrophoretic deposition is carried out under the magnetic stirring by adopting a structure of double anodes and single cathode, and the current density is set to be 3.8A/dm 2 The deposition time is 260S;
s7, putting the electroplated material into an SX4-10 box type resistance furnace, heating to 500 ℃ at a heating rate of 10 ℃/min, and preserving heat for 7min to obtain the prepared material.
Comparative example 1: no Al is added in step S4 2 O 3 The sol was otherwise the same as in example 1.
Comparative example 2: in step S4, the cubic boron nitride suspension was not added, and the rest was the same as in example 1.
Comparative example 3: in step S4, Al is not added 2 O 3 Sol and cubic boron nitride suspension, the rest being the same as in example 1.
To evaluate the wear resistance of the coatings prepared in the examples and comparative examples, we performed the following method for wear resistance testing:
the test piece was subjected to a normal temperature reciprocating abrasion test on a wheel type abrasive abrasion tester. Processing a test sample into a size of 40mm multiplied by 30mm multiplied by 4mm, selecting a positive pressure of 30N in the test, grinding a grinding piece into sand paper with a grain diameter of 180 meshes, enabling the rotating speed of a friction wheel to be 160mm/r, enabling the sample to be sensitively and repeatedly ground for one time, rotating the friction wheel for 0.9 degrees to ensure that the test sample is contacted with fresh SiC sand paper in the next cycle, rotating the friction wheel for one circle just after the test sample is ground for 400 times in the cycle, and then replacing the new SiC sand paper (the grinding grain is 80 mu m) for the next cycle. Each 400 cycles of the test specimen corresponds to 24m of rubbing travel, and each test specimen is ground in pairs 2000 times in a reciprocating manner, i.e. the total rubbing travel is 120 m. The wear resistance of the coating is evaluated by a weight loss method, the sample is subjected to ultrasonic cleaning and drying in acetone before and after each round of test, the weight loss of the sample is measured by an analytical balance with the precision of 0.1mg, and the average value of the weight loss after 5 times is taken.
FIG. 1 is a graph of the wear resistance of coatings prepared according to example 1 of the present invention and comparative examples 1-3, the specific data of which are shown in Table 1. From the figure we can see that relative to no Al addition 2 O 3 Sol and cubic boron nitride suspension, comparative example 1 or 2 with single nanoparticle addition, the wear resistance was better when Al was added simultaneously 2 O 3 After sol and cubic boron nitride suspension, the wear resistance of the material is further improved, which shows that Al 2 O 3 Certain synergistic effect exists between the sol and the cubic boron nitride suspension, and the sol and the cubic boron nitride suspension jointly promote the wear resistance of the material. We hypothesize that Al is added 2 O 3 Besides being used as a bridge between a coating and a substrate, the sol and the cubic boron nitride suspension can relieve the difference in thermal expansion coefficient between the coating and the substrate, and can improve the wear resistance of the surface of the material.
TABLE 1
Figure BDA0003709440930000061
Example 2
S1, weighing a certain amount of medicine, and adding the medicine into deionized water to dissolve the medicine to prepare the main electroplating solution, wherein the specific concentration is as follows: 180g/L of nickel chloride, 38g/L of boric acid, 35g/L of sodium hypophosphite and 0.85g/L of sodium citrate;
s2, weighing a certain amount of 9.6g aluminum isopropoxide solid by using an electronic balance, putting the weighed aluminum isopropoxide solid in a grinding dish to grind aluminum isopropoxide into powder, putting 250mL deionized water on a constant-temperature magnetic stirrer platform to heat, adding the refined aluminum isopropoxide powder to stir at a certain rotating speed when the water temperature reaches 85 ℃, setting the rotating speed to be 300r/min, stirring for 3 hours, dripping 0.625mL nitric acid into the solution while stirring, continuing to stir for a period of time, adjusting the water bath temperature to 75 ℃ after stirring, standing for 8 hours at a constant temperature, and obtaining Al with good stability and high transparency 2 O 3 Sol;
s3, placing a certain amount of deionized water into a colorimetric tube, adding a proper amount of nonionic surfactant sodium dodecyl sulfate with the concentration of 0.085g/L, carrying out ultrasonic oscillation to uniformly disperse the deionized water, weighing a certain amount of cubic boron nitride with the concentration of 3.5g/L, adding the cubic boron nitride into the deionized water, alternately carrying out eddy current mixing and ultrasonic oscillation for several times until powdery cubic boron nitride cannot be seen in a suspended emulsion in the colorimetric tube, measuring the quantitatively dispersed suspended emulsion, placing the suspended emulsion in a small beaker, dropwise adding a small amount of electroplating main solution under the mechanical stirring action, and stirring uniformly;
s4, placing the electroplating solution prepared in the step S1 on a magnetic stirrer, and stirring the electroplating solution according to the proportion of 2: 0.8: 97.2 by volume was gradually and slowly added to the Al prepared in steps S2 and S3 2 O 3 Sol and cubic boron nitride suspension;
s5, polishing the small steel sheet by using sand paper to remove a surface oxidation film, and then carrying out chemical degreasing and acid washing activation, wherein the chemical degreasing solution mainly comprises the following components in percentage by weight: 58g/L of sodium hydroxide, 32g/L of sodium carbonate, 47g/L of sodium phosphate and 6.9g/L of sodium silicate, wherein the acid-washing solution mainly comprises the following components in percentage by weight: 26mL/L hydrochloric acid with the concentration of 1.05g/mL and 54 mL/L35% hydrofluoric acid, and the specific implementation steps comprise placing the small steel sheet in the solution, and carrying out ultrasonic treatment for a period of time, wherein the chemical oil removal time is 23min, and the acid cleaning activation time is 270 s;
and S6, wiping the pretreated matrix, and placing the matrix in a self-made electrophoresis tank. The nickel sheet is used as anode, the stainless steel sheet is used as cathode, the structure of double anode and single cathode is adopted for electrophoretic deposition under magnetic stirring, and the current density is set to be 3.8A/dm 2 The deposition time is 260S;
s7, putting the electroplated material into an SX4-10 box type resistance furnace, heating to 500 ℃ at a heating rate of 10 ℃/min, and preserving heat for 7min to obtain the prepared material.
Comparative example 4: in step S1, sodium hypophosphite was not added, and the rest was the same as in example 2.
Comparative example 5: in step S1, sodium citrate was not added, and the rest was the same as in example 2.
Comparative example 6: in step S1, sodium hypophosphite and sodium citrate were not added, and the rest was the same as in example 2.
Fig. 2 is a scanned graph of the preparation of example 2 and comparative examples 3-5 of the present invention, from which we can clearly see that example 2 is smoother compared to comparative examples 3-5, which shows that the Na and P elements can promote the uniformity of the plating layer, because the Na and P elements can form an irregular continuous network frame between the plating layers, which has an important significance for the uniformity of the plating layer surface.
Example 3
S1, weighing a certain amount of medicine, and adding the medicine into deionized water to dissolve the medicine to prepare the main electroplating solution, wherein the specific concentration is as follows: 180g/L of nickel chloride, 38g/L of boric acid, 35g/L of sodium hypophosphite and 0.85g/L of sodium citrate;
s2, weighing a certain amount of 9.6g aluminum isopropoxide solid by using an electronic balance, putting the weighed aluminum isopropoxide solid in a grinding dish to grind aluminum isopropoxide into powder, putting 250mL deionized water on a constant-temperature magnetic stirrer platform to heat, adding the refined aluminum isopropoxide powder to stir at a certain rotating speed when the water temperature reaches 85 ℃, setting the rotating speed to be 300r/min, stirring for 3 hours, dripping 0.625mL nitric acid into the solution while stirring, continuing to stir for a period of time, adjusting the water bath temperature to 75 ℃ after stirring, standing for 8 hours at a constant temperature, and obtaining Al with good stability and high transparency 2 O 3 Sol;
s3, placing a certain amount of deionized water into a colorimetric tube, adding a proper amount of non-ionic surfactant sodium dodecyl sulfate with the concentration of 0.085g/L, carrying out ultrasonic oscillation to uniformly disperse the deionized water, weighing a certain amount of cubic boron nitride with the concentration of 3.5g/L, adding the weighed cubic boron nitride into the deionized water, alternately carrying out eddy current uniform mixing and ultrasonic oscillation for a plurality of times until powdery cubic boron nitride cannot be seen in a suspended emulsion in the colorimetric tube, measuring the quantitatively dispersed suspended emulsion, placing the measured suspended emulsion into a small beaker, dropwise adding a small amount of electroplating main solution under the mechanical stirring action, and stirring uniformly;
s4, placing the electroplating solution prepared in the step S1 on a magnetic stirrer, and stirring the electroplating solution according to the proportion of 1.5: 1.3: 97.2 by volume, Al prepared in steps S2 and S3 was gradually and slowly added 2 O 3 Sol and cubic boron nitride suspension;
s5, polishing the small steel sheet by using sand paper to remove a surface oxidation film, and then carrying out chemical degreasing and acid washing activation, wherein the chemical degreasing solution mainly comprises the following components: 58g/L of sodium hydroxide, 32g/L of sodium carbonate, 47g/L of sodium phosphate and 6.9g/L of sodium silicate, wherein the acid-washing solution mainly comprises the following components in percentage by weight: 26mL/L hydrochloric acid with the concentration of 1.05g/mL and 54 mL/L35% hydrofluoric acid, and the specific implementation steps comprise placing the small steel sheet in the solution, and carrying out ultrasonic treatment for a period of time, wherein the chemical oil removal time is 23min, and the acid cleaning activation time is 270 s;
and S6, wiping the pretreated matrix, and placing the matrix in a self-made electrophoresis tank. Taking a nickel sheet as an anode and a stainless steel sheet as a cathodePerforming electrophoretic deposition under magnetic stirring by using a structure of double anodes and single cathode, wherein the current density is set to be 3.8A/dm 2 The deposition time is 260S;
s7, putting the electroplated material into an SX4-10 box type resistance furnace, heating to 500 ℃ at a heating rate of 10 ℃/min, and preserving heat for 7min to obtain the prepared material.
Comparative example 7: the acid washing activation time in step S5 was 170 seconds, and the rest was the same as in example 2.
Comparative example 8: the acid washing activation time in step S5 was 370S, and the rest was the same as in example 2.
To evaluate the corrosion resistance of the coatings prepared in the examples and comparative examples, we performed the following method for corrosion resistance testing:
the test uses CHI660B electrochemical workstation produced by Shanghai Chenhua company, and carries out electrochemical full-immersion corrosion test on the sample in 3.5% NaCl solution to obtain the polarization curve of the brush plating layer under corresponding process parameters, and the corrosion performance of the brush plating layer is represented by two parameters of corrosion potential and corrosion current density. A three-electrode system is adopted in the test, a reference electrode is a saturated calomel electrode, an auxiliary electrode is a platinum wire, and a working electrode is a plating layer sample to be tested. Before the test, the corroded part of the brush plating layer is fully contacted with a corrosion medium, the corrosion medium is kept for about 10min, the test is started after the system state is stable, the scanning speed is 2mV/s, and the scanning interval is-1.0-0.5V. And evaluating the corrosion resistance of the brush plating layer by adopting a polarization curve (Tafel curve) and corresponding corrosion potential and corrosion current density.
FIG. 3 is a polarization diagram of examples 1 to 3 and comparative examples 7 to 8, and it is seen from the graphs that the corrosion resistances of examples 1 to 3 and comparative examples 7 to 8 are different, and in general, the more positive the corrosion potential, the less susceptible to corrosion, the lower the corrosion current density, the slower the corrosion rate, and the stronger the corrosion resistance. From the polarization curve parameters, it can be seen that the corrosion current density of example 2 is at the minimum and the corrosion potential is at the most negative, and the corrosion potential and the corrosion current density of example 2 are inferior, but considering both parameters, the corrosion resistance is the best at this time, which indicates that the proper pickling time has an accelerating effect on the corrosion resistance of the material.
In summary, the invention discloses an electroplating process, which utilizes cubic boron nitride and aluminum oxide as the high-hardness nanoparticles to disperse and distribute in the matrix metal, not only improves the hardness of the plating layer, but also can effectively separate the corrosion medium from the matrix metal, reduce the area of the matrix metal exposed in the corrosion solution, and prevent the further corrosion of the plating layer by the corrosion solution. Meanwhile, the added Na and P elements can play a synergistic effect with the nano particles, so that the microstructure of the coating is obviously improved, the bonding force between the substrate metal and the ceramic base layer is enhanced, and the corrosion resistance of the material is further improved. In addition, the acid washing activation time of the base material is prolonged, the binding force with the coating is improved by manufacturing a rough base surface, the effects of phase change and brittle fracture of the coating and the base material caused by the difference of expansion coefficients are weakened, and the process plays an important role in corrosion prevention of the water pump pull rod.
The above-mentioned embodiments only express the specific embodiments of the present invention, and the description thereof is specific and detailed, but not construed as limiting the scope of the present invention. It should be understood that any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principles of the invention should be construed as equivalents thereof, which should be construed by those skilled in the art and are within the scope of the invention.

Claims (9)

1. An electroplating method for improving the corrosion resistance of a water pump pull rod is characterized in that: the method comprises the following specific steps:
s1, weighing a certain amount of medicine, and adding the medicine into deionized water to dissolve the medicine to prepare the main electroplating solution, wherein the specific concentration is as follows: the concentration of nickel chloride is 140-260g/L, the concentration of boric acid is 33-46g/L, the concentration of sodium hypophosphite is 23-48g/L, and the concentration of sodium citrate is 0.35-0.96 g/L;
s2, weighing a certain amount of 8-16g of aluminum isopropoxide solid by using an electronic balance, putting the weighed aluminum isopropoxide solid in a grinding dish to grind the aluminum isopropoxide into powder, putting 250mL of deionized water on a constant-temperature magnetic stirrer platform to heat, wherein the water temperature isAdding refined isopropanol aluminum powder at a certain rotation speed when the temperature reaches 85 ℃, stirring, dripping a certain amount of nitric acid into the solution while stirring, continuously stirring for a period of time, adjusting the temperature of a water bath kettle to 50-90 ℃, standing for 5-15h at a constant temperature, and obtaining Al with good stability and high transparency 2 O 3 Sol;
s3, placing a certain amount of deionized water into a colorimetric tube, adding a proper amount of nonionic surfactant sodium dodecyl sulfate with the concentration of 0.05-0.15g/L, carrying out ultrasonic oscillation to uniformly disperse the deionized water, weighing a certain amount of cubic boron nitride with the concentration of 5-25g/L, adding the weighed cubic boron nitride into the deionized water, alternately carrying out eddy current uniform mixing and ultrasonic oscillation for several times until powdery cubic boron nitride cannot be seen in the suspended emulsion in the colorimetric tube, weighing the fixed amount of dispersed suspended emulsion, placing the suspended emulsion in a small beaker, dropwise adding a small amount of electroplating main solution under the action of mechanical stirring, and stirring uniformly;
s4, placing the electroplating solution prepared in the step S1 on a magnetic stirrer, and gradually and slowly adding the Al prepared in the steps S2 and S3 according to a certain volume ratio under the action of mechanical stirring 2 O 3 Sol and cubic boron nitride suspension;
s5, polishing the small steel sheet by using sand paper to remove a surface oxidation film, and then carrying out chemical degreasing and acid washing activation, wherein the chemical degreasing solution mainly comprises the following components in percentage by weight: 35-96g/L of sodium hydroxide, 12-65g/L of sodium carbonate, 35-67g/L of sodium phosphate and 2.5-9.6g/L of sodium silicate, wherein the acid-washing solution mainly comprises the following components in percentage by weight: 18-46mL/L hydrochloric acid with the concentration of 1.05g/mL and 36-78 mL/L35% hydrofluoric acid, and the specific implementation steps comprise placing a small steel sheet in the solution, and carrying out ultrasonic treatment for a period of time;
and S6, wiping the pretreated matrix, and placing the matrix in a self-made electrophoresis tank. The nickel sheet is used as an anode, the stainless steel sheet is used as a cathode, the electrophoretic deposition is carried out under the magnetic stirring by adopting a structure of double anodes and single cathode, and the current density is set to be 3-8A/dm 2 The deposition time is 160-380S;
s7, putting the electroplated material into an SX4-10 box type resistance furnace, heating to a specific temperature according to a certain heating rate, and preserving the temperature for a period of time to obtain the prepared material.
2. The electroplating method for improving the corrosion resistance of the water pump pull rod according to claim 1, characterized in that: 180g/L of nickel chloride, 38g/L of boric acid, 35g/L of sodium hypophosphite and 0.85g/L of sodium citrate in the S1.
3. The electroplating method for improving the corrosion resistance of the water pump pull rod according to claim 1, characterized in that: 160g/L of nickel chloride, 35g/L of boric acid, 28g/L of sodium hypophosphite and 0.67g/L of sodium citrate in the S1.
4. The electroplating method for improving the corrosion resistance of the water pump pull rod according to the claim 2 or 3, is characterized in that: and the mass of the aluminum isopropoxide solid in the S2 is 9.6g, and the temperature of the water bath is maintained for 8h at 75 ℃.
5. The electroplating method for improving the corrosion resistance of the water pump pull rod according to claim 4, wherein the electroplating method comprises the following steps: the concentration of the sodium dodecyl sulfate in the S3 is 0.085g/L, and the concentration of the cubic boron nitride is 12 g/L.
6. The electroplating method for improving the corrosion resistance of the water pump pull rod according to claim 4, wherein the electroplating method comprises the following steps: the concentration of sodium dodecyl sulfate in the S3 is 0.12g/L, and the concentration of cubic boron nitride is 18 g/L.
7. The electroplating method for improving the corrosion resistance of the water pump pull rod according to claim 5 or 6, characterized in that: the formula of the solution for chemical degreasing in S5 is as follows: 58g/L of sodium hydroxide, 32g/L of sodium carbonate, 47g/L of sodium phosphate and 6.9g/L of sodium silicate, and the acid cleaning solution comprises 26mL/L of hydrochloric acid with the concentration of 1.05g/mL and 54mL/L of 35% hydrofluoric acid.
8. The electroplating method for improving the corrosion resistance of the water pump pull rod according to claim 5 or 6, characterized in that: the formula of the solution for chemical degreasing in S5 is as follows: 67g/L of sodium hydroxide, 48g/L of sodium carbonate, 56g/L of sodium phosphate and 7.8g/L of sodium silicate, and the formula of the acid-washed solution comprises 35mL/L of hydrochloric acid with the concentration of 1.05g/mL and 69mL/L of 35% hydrofluoric acid.
9. An electroplating method for improving the corrosion resistance of a water pump pull rod according to claim 7 or 8, characterized in that: the acid washing activation time in the S5 is 120S.
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