CN114892241A - High-temperature wear-resistant Ni-Mo-based nitride ceramic phase composite coating and preparation method thereof - Google Patents
High-temperature wear-resistant Ni-Mo-based nitride ceramic phase composite coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-temperature wear-resistant Ni-Mo based nitride ceramic phase composite coating, which comprises the following steps: step S1, mechanically preprocessing the substrate to make the surface smooth; then degreasing and ultrasonic cleaning are carried out on the surface of the oxide layer, and activation treatment is carried out to remove the oxide layer. And step S2, taking graphite as an anode, and depositing a Ni-Mo coating in the nickel ion-molybdate-citrate system electroplating solution by adopting direct current. And step S3, adding urea solution containing nitride ceramic phase particles into the plating solution in the direct current electrodeposition process, and stirring at a high speed of 300 r/min to prepare the deposited Ni-Mo based nitride ceramic phase composite coating. And S4, carrying out vacuum heat treatment on the coating obtained in the step S3 to obtain the annealed Ni-Mo based nitride ceramic phase composite coating. The method has the advantages of simple operation, easy control of conditions and good repeatability, and the composite coating has good high-temperature hardness and wear resistance.
Description
Technical Field
The invention belongs to the technical field of alloy coating preparation and application, relates to a high-temperature wear-resistant Ni-Mo based nitride ceramic phase composite coating and a preparation method thereof, and particularly relates to preparation of a Ni-Mo based composite coating which takes Ni and Mo as main elements and contains one or more nitride ceramic phases.
Background
With the progress of industrialization, in the past, Cr plating is mainly used in the traditional industry, and the traditional Cr plating technology is gradually eliminated due to the defects of toxicity, high waste liquid treatment cost and the like. At present, the Ni-Mo based plating layer enters the visual field of people with the advantages of high comprehensive performance, convenient and fast operation and the like. And the composite plating layer made of Ni and other alloys can be made into plating layers with different functionalities through a plating solution formula, so that the research on the relevant preparation process and performance of the Ni-Mo based plating layer has great application development space and prospect. Although Ni-based coatings have certain advantages over Cr-based coatings, with the development of modernization, binary Ni-Mo-based alloys have not been able to meet certain requirements of scientific production, so we often use composite electrodeposition to surface modify parts. Composite electrodeposition is a surface protection technique for obtaining functional coatings. The nickel-based composite coating which is stable in the atmospheric environment can be prepared by the composite electrodeposition method, and compared with a film prepared by a single-phase electrodeposition method, the film has stronger passivation capability, higher hardness and brighter surface, so that the surface performance of the material is effectively improved, and certain economic benefits can be generated in the aspects of decorative coating and the like. One or more nitride ceramic phases are used as dispersed particles to prepare the Ni-Mo based composite coating, so that the wear resistance of the coating can be further improved to achieve the purpose of repairing the surface of a part.
Disclosure of Invention
The invention aims to solve the defects of the prior art and provides a preparation method of a high-temperature wear-resistant Ni-Mo based nitride ceramic phase composite coating, the process is simple to operate, the conditions are easy to control, the repeatability is good, the prepared deposition coating is well combined with a matrix, the film forming quality is good, and the hardness and the wear resistance are good at high temperature.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the high-temperature wear-resistant Ni-Mo based nitride ceramic phase composite coating comprises the following steps:
step S1, mechanically preprocessing the substrate to make the surface smooth; then, degreasing and ultrasonic cleaning are carried out on the surface of the substrate by using a commercial degreasing agent, and the surface of the substrate is activated to remove an oxide layer.
And step S2, taking graphite as an anode, and depositing a Ni-Mo coating in the nickel ion-molybdate-citrate system electroplating solution by adopting direct current.
And step S3, adding urea solution containing nitride ceramic phase particles into the plating solution and stirring at a high speed of 300 r/min in the process of electrodepositing the Ni-Mo coating by S2 to prepare the deposited Ni-Mo based nitride ceramic phase composite coating.
And S4, carrying out vacuum heat treatment on the coating obtained by the deposition of the S3 to obtain the final annealed Ni-Mo based nitride ceramic phase composite coating.
Preferably, the substrate is one of brass sheet, stainless steel or low carbon steel; the ultrasonic cleaning time is 5-25 min, and the activating solution is dilute hydrochloric acid or dilute sulfuric acid with volume fraction of 5-15%.
Preferably, the nickel ion-molybdate-citrate system electroplating solution described in the step S2 includes 20 to 120 g/L of nickel sulfate, 5 to 80g/L of sodium molybdate, 5 to 40 g/L of ammonium chloride, 5 to 60 g/L of sodium carbonate, 30 to 150 g/L of sodium citrate, 0.02 to 0.25 g/L of sodium dodecyl sulfate, and 0.5 to 3 g/L of saccharin sodium. The direct current deposition current density is 1-4.5A/dm 2 The deposition time is 5-30 min.
Preferably, the urea solution of step S3 is a mixed solution containing urea and nitride ceramic phase particles, the pH of the mixed solution is 3.5-7.5 after mixing with the plating solution of step S2, the deposition time is 2-25 min, and the nitride ceramic phase particles are BN ceramic phase particles, TiN ceramic phase particles, AlN ceramic phase particles, Si ceramic phase particles 3 N 4 Ceramic phase particles, ZrN 2 One or more of ceramic phase particles. The concentration of each component in the urea solution is respectively as follows: 0-20 g/L of urea and not 0; 0-30 g/L, TiN g/0-30 g/L, AlN g/0-30 g/L, Si g/0 g/3878 g ceramic phase particle 3 N 4 0-30 g/L, ZrN g of ceramic phase particles 2 0-30 g/L of ceramic phase particles, and not 0 at the same time.
Preferably, the vacuum heat treatment of the deposited coating in step S4 is specifically: raising the temperature to 400-; the temperature rise time was 60 min.
Preferably, the high-hardness ceramic phase is preferably contained in the composite coating layer in an amount in the range of 10% or less.
According to the preparation method of the high-temperature wear-resistant Ni-Mo based nitride ceramic phase composite coating, the surface of the Ni-Mo based nitride ceramic phase composite coating prepared by the electrodeposition method is uniform and compact, no obvious crack and pore defects exist, and the film layer and the matrix have good bonding property. The nitride ceramic phase nano particles are uniformly dispersed in the Ni-Mo alloy plating layer, but the deposition amount of the nitride ceramic phase on the surface of the substrate is increased and then decreased along with the increase of the addition amount of the nitride ceramic phase in the plating solution. The addition of the nitride ceramic phase particles can play a certain grain refining role on the coating, and the refining effect is more obvious compared with that of the Ni-Mo film after the annealing at the temperature of 600 ℃. The strengthening of the film layer at 600 deg.c is caused by the grain refinement and the combined action of other precipitated phases after mutual diffusion. The nitride ceramic phase nano-particles can improve the wear resistance of the Ni-Mo based composite coating by improving the hardness of the film. Meanwhile, a certain antifriction effect is achieved through the self-lubricating property of partial nitride ceramic phase particles. Particularly, with the increase of the annealing temperature, when the temperature reaches 600 ℃, the friction mechanism is changed from adhesive wear to abrasive wear, and the wear resistance and the anti-friction wear resistance are obviously improved.
From the aspects of raw materials, preparation process and product structure, the invention has the following advantages:
1. the process has the advantages of simple operation, easily controlled conditions and good repeatability.
2. The prepared deposition coating has good combination with the matrix and good film forming quality.
3. The obtained coating has good hardness and wear resistance at high temperature.
4. The coating uses Ni-Mo as a main element, and the thermal stability of the Ni-Mo based coating structure is improved by adding nitride ceramic phase particles, so that the coating has good heat resistance.
Drawings
FIG. 1 is a parameter diagram of a coating heat treatment process;
FIG. 2 is a surface SEM image of Ni-Mo-BN coatings prepared in examples 1-4;
FIG. 3 is XRD diffraction pattern of Ni-Mo-BN coatings prepared by examples 2, 5 and 6: (a) example 2; (b) example 5; (c) example 6;
FIG. 4 is a graph of the coefficient of friction of the coatings prepared in examples 2, 5, 6 versus time.
Detailed Description
It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the disclosure.
The present invention is further illustrated by the following specific examples, which are not intended to limit the scope of the invention. The examples, where specific techniques and reaction conditions are not indicated, can be carried out according to the techniques or conditions or product specifications described in the literature in the field. Reagents, instruments or equipment of any manufacturer not indicated are commercially available.
Example 1
Mechanically pretreating the brass sheet to make the surface of the brass sheet smooth; and then degreasing and ultrasonically cleaning the surface of the brass sheet for 10 min by using a commercial degreasing agent, and activating the surface of the brass sheet by using dilute sulfuric acid with the volume fraction of 10% to remove an oxide layer. Graphite is used as an anode, and a current density of 2A/cm is adopted in an electroplating solution containing 60 g/L of nickel sulfate, 10 g/L of sodium molybdate, 10 g/L of ammonium chloride, 10 g/L of sodium carbonate, 80g/L of sodium citrate, 0.1 g/L of sodium dodecyl sulfate and 1.5 g/L of saccharin sodium 2 Depositing the Ni-Mo coating by direct current, adding 10 g/L urea and 5 g/L BN ceramic particle phase into the plating solution after beginning to deposit for 5 min, and stirring at a high speed of 300 r/min to deposit and obtain the Ni-Mo-BN composite coating. And drying the coating obtained by deposition to remove water, and performing heat treatment at 25 ℃ for 1h to obtain the Ni-Mo-BN composite coating with the BN content of 1.2 wt.%.
Example 2
Mechanically pretreating the brass sheet to make the surface of the brass sheet smooth; then, degreasing and ultrasonic cleaning are carried out on the surface of the brass sheet for 10 min by using a commercial degreasing agent, and activation treatment is carried out on the surface of the brass sheet by using dilute sulfuric acid with the volume fraction of 10% to remove an oxidation layer. Graphite is used as an anode, and a current density of 2A/cm is adopted in an electroplating solution containing 60 g/L of nickel sulfate, 10 g/L of sodium molybdate, 10 g/L of ammonium chloride, 10 g/L of sodium carbonate, 80g/L of sodium citrate, 0.1 g/L of sodium dodecyl sulfate and 1.5 g/L of saccharin sodium 2 Depositing the Ni-Mo coating by direct current, adding 10 g/L urea and 10 g/L BN ceramic particle phase into the plating solution after 5 min of deposition, stirring at a high speed of 300 r/min, and depositing to obtain the Ni-Mo-BN composite coating. Drying the coating obtained by deposition to remove water, and carrying out heat treatment for 1h at 25 ℃ to obtain the Ni-Mo-BN composite coatingBN content 2.6 wt.%.
Example 3
Mechanically pretreating the brass sheet to make the surface of the brass sheet smooth; then, degreasing and ultrasonic cleaning are carried out on the surface of the brass sheet for 10 min by using a commercial degreasing agent, and activation treatment is carried out on the surface of the brass sheet by using dilute sulfuric acid with the volume fraction of 10% to remove an oxidation layer. Graphite is used as an anode, and a current density of 2A/cm is adopted in an electroplating solution containing 60 g/L of nickel sulfate, 10 g/L of sodium molybdate, 10 g/L of ammonium chloride, 10 g/L of sodium carbonate, 80g/L of sodium citrate, 0.1 g/L of sodium dodecyl sulfate and 1.5 g/L of saccharin sodium 2 Depositing the Ni-Mo coating by direct current, adding 10 g/L urea and 15 g/L BN ceramic particle phase into the plating solution after beginning to deposit for 5 min, and stirring at a high speed of 300 r/min to deposit and obtain the Ni-Mo-BN composite coating. And drying the coating obtained by deposition to remove water, and performing heat treatment at 25 ℃ for 1h to obtain the Ni-Mo-BN composite coating with the BN content of 3.2 wt.%.
Example 4
Mechanically pretreating the brass sheet to make the surface of the brass sheet smooth; then, degreasing and ultrasonic cleaning are carried out on the surface of the brass sheet for 10 min by using a commercial degreasing agent, and activation treatment is carried out on the surface of the brass sheet by using dilute sulfuric acid with the volume fraction of 10% to remove an oxidation layer. Graphite is used as an anode, and a current density of 2A/cm is adopted in an electroplating solution containing 60 g/L of nickel sulfate, 10 g/L of sodium molybdate, 10 g/L of ammonium chloride, 10 g/L of sodium carbonate, 80g/L of sodium citrate, 0.1 g/L of sodium dodecyl sulfate and 1.5 g/L of saccharin sodium 2 Depositing the Ni-Mo coating by direct current, adding 10 g/L urea and 20 g/L BN ceramic particle phase into the plating solution after beginning to deposit for 5 min, and stirring at a high speed of 300 r/min to deposit and obtain the Ni-Mo-BN composite coating. And drying the coating obtained by deposition to remove water, and performing heat treatment at 25 ℃ for 1h to obtain the Ni-Mo-BN composite coating with the BN content of 2.1 wt.%.
Example 5
Mechanically pretreating the brass sheet to make the surface of the brass sheet smooth; then, degreasing and ultrasonic cleaning are carried out on the surface of the brass sheet for 10 min by using a commercial degreasing agent, and activation treatment is carried out on the surface of the brass sheet by using dilute sulfuric acid with the volume fraction of 10% to remove an oxidation layer. Graphite is used as an anode, and the anode comprises 60 g/L nickel sulfate, 10 g/L sodium molybdate,10 g/L of ammonium chloride, 10 g/L of sodium carbonate, 80g/L of sodium citrate, 0.1 g/L of sodium dodecyl sulfate and 1.5 g/L of saccharin sodium are adopted in electroplating solution with current density of 2A/cm 2 Depositing the Ni-Mo coating by direct current, adding 10 g/L urea and 10 g/L BN ceramic particle phase into the plating solution after 5 min of deposition, stirring at a high speed of 300 r/min, and depositing to obtain the Ni-Mo-BN composite coating. And drying the coating obtained by deposition to remove moisture, and carrying out vacuum heat treatment at 400 ℃ for 1h to obtain the Ni-Mo-BN composite coating with the BN content of 2.6 wt.% in the annealing state at 400 ℃.
Example 6
Mechanically pretreating the brass sheet to make the surface of the brass sheet smooth; then, degreasing and ultrasonic cleaning are carried out on the surface of the brass sheet for 10 min by using a commercial degreasing agent, and activation treatment is carried out on the surface of the brass sheet by using dilute sulfuric acid with the volume fraction of 10% to remove an oxidation layer. Graphite is used as an anode, and a current density of 2A/cm is adopted in an electroplating solution containing 60 g/L of nickel sulfate, 10 g/L of sodium molybdate, 10 g/L of ammonium chloride, 10 g/L of sodium carbonate, 80g/L of sodium citrate, 0.1 g/L of sodium dodecyl sulfate and 1.5 g/L of saccharin sodium 2 Depositing the Ni-Mo coating by direct current, adding 10 g/L urea and 10 g/L BN ceramic particle phase into the plating solution after 5 min of deposition, stirring at a high speed of 300 r/min, and depositing to obtain the Ni-Mo-BN composite coating. And drying the coating obtained by deposition to remove moisture, and carrying out vacuum heat treatment at 600 ℃ for 1h to obtain the Ni-Mo-BN composite coating with the BN content of 2.6 wt.% in the 600 ℃ annealing state.
See table 1 for details.
As can be seen from the above table, the Ni — Mo based nitride ceramic phase composite coatings obtained in examples 2, 5, and 6 sequentially increased with the annealing temperature, and the friction coefficient of the coating increased and decreased with the hardness of the coating decreased, the wear loss decreased, and the high temperature wear resistance of the coating increased.
Examples 1-4 show that the BN content of the coating surface increases with increasing BN ceramic phase addition, which contributes to the increase in coating hardness and wear resistance, as shown in table 1.
Other embodiments of the invention will be apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. This application is intended to cover any variations, uses, or adaptations of the invention following, in general, the principles of the invention and including such departures from the present disclosure as come within known or customary practice within the art to which the invention pertains. It is intended that the specification and examples be considered as exemplary only, with a true scope and spirit of the invention being indicated by the following claims.
It is to be understood that the present invention is not limited to what has been described above, and that various modifications and changes may be made without departing from the scope thereof. The scope of the invention is limited only by the appended claims.
Claims (10)
1. A preparation method of a high-temperature wear-resistant Ni-Mo based nitride ceramic phase composite coating is characterized by comprising the following steps:
step S1, mechanically preprocessing the substrate to make the surface smooth; then degreasing and ultrasonic cleaning the surface of the substrate by using a degreasing agent, and activating the surface of the substrate to remove an oxide layer;
s2, depositing a Ni-Mo coating in a nickel ion-molybdate-citrate system electroplating solution by using direct current with graphite as an anode;
step S3, in the process of electrodepositing the Ni-Mo coating in step S2, adding urea solution containing nitride ceramic phase particles into the plating solution and stirring at a high speed of 300 r/min to prepare the deposited Ni-Mo based nitride ceramic phase composite coating.
2. And S4, carrying out vacuum heat treatment on the coating deposited in the step S3 to obtain the final annealed Ni-Mo based nitride ceramic phase composite coating, namely the high-temperature wear-resistant Ni-Mo based nitride ceramic phase composite coating.
3. The method according to claim 1, wherein the substrate of step S1 is brass sheet, stainless steel or low carbon steel; the ultrasonic cleaning time is 5-25 min, and the activating solution is dilute hydrochloric acid or dilute sulfuric acid with volume fraction of 5-15%.
4. The method according to claim 1, wherein the nickel ion-molybdate-citrate system electroplating solution in step S2 is an aqueous solution containing nickel sulfate, sodium molybdate, nickel chloride, sodium citrate, sodium lauryl sulfate and saccharin sodium.
5. The method according to claim 3, wherein the concentrations of the components in the ni-mo lybdate-citrate system plating solution are as follows: 20-120 g/L nickel sulfate, 5-80 g/L sodium molybdate, 5-40 g/L ammonium chloride, 5-60 g/L sodium carbonate, 30-150 g/L sodium citrate, 0.02-0.25 g/L sodium dodecyl sulfate and 0.5-3 g/L saccharin sodium.
6. The method according to claim 1, wherein the DC electrodeposition current in step S2 has a current density of 1 to 4.5A/dm 2 The deposition time is 5-30 min.
7. The method according to claim 1, wherein the urea solution of step S3 is a mixed solution containing urea and nitride ceramic phase particles, the mixed solution is mixed with the plating solution of step S2, the pH of the mixed solution is 3.5 to 7.5, the deposition time is 2 to 25 min, and the nitride ceramic phase particles are BN ceramic phase particles, TiN ceramic phase particles, AlN ceramic phase particles, Si ceramic phase particles 3 N 4 Ceramic phase particles, ZrN 2 One or more of ceramic phase particles.
8. The process according to claim 5, characterized in that the concentrations of the constituents of the urea solution are: 0-20 g/L of urea and not 0; 0-30 g/L, TiN g/0-30 g/L, AlN g/0-30 g/L, Si g/0 g/3878 g ceramic phase particle 3 N 4 0-30 g/L, ZrN g of ceramic phase particles 2 0-30 g/L of ceramic phase particles, and not 0 at the same time.
9. The method according to claim 1, wherein the vacuum heat treatment of step S4 is specifically: raising the temperature to 400-; the temperature rise time was 60 min.
10. A high-temperature wear-resistant Ni-Mo-based nitride ceramic phase composite coating prepared by the preparation method according to any one of claims 1 to 8.
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