CN114737184A - High-hardness nano TiC particle reinforced phosphoric acid reaction tank stirring paddle blade high-entropy alloy composite coating and preparation method thereof - Google Patents
High-hardness nano TiC particle reinforced phosphoric acid reaction tank stirring paddle blade high-entropy alloy composite coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a high-hardness nano TiC particle reinforced phosphoric acid reaction tank stirring paddle blade high-entropy alloy composite coating and a preparation method thereof, wherein the high-hardness nano TiC particle reinforced phosphoric acid reaction tank stirring paddle blade high-entropy alloy composite coating is prepared according to the following method: 1) accurately weighing FeCoCrNi high-entropy alloy powder and TiC particles; 2) placing FeCoCrNi high-entropy alloy powder and TiC particles into a ball milling tank for ball milling to ensure that the powder is uniformly mixed, and then sieving, drying and storing; 3) selecting a 904L stainless steel plate as a base material, removing surface oxide skin, cleaning off surface oil stains, and drying for later use; 4) a layer of powder is preset on the surface of a base material by a stainless steel die by a powder prefabricating method, the base material is compacted by a stainless steel knife, a coating is prepared by broadband laser cladding, and argon is introduced for protection in the cladding process. The hardness, the wear resistance and the corrosion resistance of the high-entropy alloy are improved. Provides a high wear-resistant and corrosion-resistant material formula and a surface coating preparation technology for the phosphorus chemical industry in China.
Description
Technical Field
The invention relates to the technical field of alloys, in particular to a high-entropy alloy composite coating of a high-hardness nano TiC particle reinforced phosphoric acid reaction tank stirring paddle blade and a preparation method thereof.
Background
China is a large country for phosphorus chemical industry production in the world, and the specific gravity of the yield of phosphorus chemical industry products (such as phosphoric acid, chemical fertilizers and the like) in the total yield in the world is large. Phosphoric acid produced by phosphorus chemical enterprises is obtained by the replacement reaction of sulfuric acid and phosphate ore. In the production process of phosphoric acid, the blades of the stirring paddle and phosphate ore are strongly collided, and severe erosion corrosion occurs. 904L of super austenitic stainless steel is generally adopted in the prior stirring paddle blade, although the super austenitic stainless steel has enough strong acid corrosion resistance, the hardness is low (about 190HV), the abrasion resistance is poor, the service life is only 8 months, the annual repair cost is over hundred million yuan, and the phosphorization industry urgently needs high abrasion resistance and corrosion resistance substitute materials.
The high-entropy alloy can achieve both wear resistance and corrosion resistance through component regulation and control, and is hopeful to be used as a substitute material. The high-entropy alloy is also called multi-component alloy, generally comprises 5-13 elements, and is obtained by metal or nonmetal with equal atomic ratio or unequal atomic ratio according to a certain preparation technology. High entropy alloys were first proposed in 2004 by professor yesterday of scholars in taiwan, china. The appearance of the novel material provides a new idea for developing a new material.
The high-entropy alloy has a plurality of properties superior to those of the traditional Fe, Ti and Ni-based alloy, such as simple solid solution structure and excellent high-temperature structure stability on the structure, high strength and hardness, excellent corrosion resistance and wear resistance and the like on the performance, and has wide application prospect in the fields of cutters for high-speed cutting, various tools and dies, turbine blades and the like.
High entropy alloys generally consist of FCC, BCC or HCP simple solid solutions with little formation of intermetallic compounds. The high-entropy alloy has unique high-entropy effect, lattice distortion effect, delayed diffusion effect and cocktail effect, so that the high-entropy alloy shows excellent performances such as high strength and hardness, wear resistance, corrosion resistance and the like. The ceramic reinforcing phase is beneficial to improving the capabilities of work hardening, fine grain strengthening, precipitation strengthening and the like of the high-entropy alloy, thereby effectively improving the hardness and the wear resistance of the high-entropy alloy. The design of the high-entropy alloy coating suitable for repairing the blades of the stirring paddle in the phosphorus chemical industry is a problem which needs to be solved urgently at present in the phosphorus chemical industry.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a preparation method of a high-entropy alloy composite coating of a high-hardness nano TiC particle reinforced phosphoric acid reaction tank stirring paddle blade, and the second aim is to provide the high-entropy alloy coating prepared by the method, so that the hardness, the wear resistance and the corrosion resistance of the high-entropy alloy are improved.
In order to achieve the first purpose, the invention adopts the following technical scheme: a preparation method of a high-entropy alloy composite coating of high-hardness nano TiC particle reinforced phosphoric acid reaction tank stirring paddle blades is characterized by comprising the following steps:
1) accurately weighing FeCoCrNi high-entropy alloy powder and TiC particles;
2) placing FeCoCrNi high-entropy alloy powder and TiC particles into a ball milling tank for ball milling to ensure that the powder is uniformly mixed, and then sieving, drying and storing;
3) selecting a 904L stainless steel plate as a base material, removing surface oxide skin, cleaning surface oil stains, and drying for later use;
4) a layer of powder is preset on the surface of a base material by a stainless steel die by a powder prefabricating method, the base material is compacted by a stainless steel knife, a coating is prepared by broadband laser cladding, and argon is introduced for protection in the cladding process.
In the scheme, the method comprises the following steps: the addition amount of TiC is 5-12.5 vol%.
In the scheme, the method comprises the following steps: the FeCoCrNi high-entropy alloy powder is spherical powder with the size of 45-105 mu m and the purity of 99.0-99.5%, the TiC powder is irregular granular, the particle size is 5-15 mu m, and the powder purity is more than or equal to 99.5%.
In the scheme, the method comprises the following steps: the ball milling parameters are that the ball material ratio is 5: 1, ball milling rotation speed of 250-.
In the scheme, the method comprises the following steps: and sieving the ball-milled powder by a 120-mesh stainless steel sample sieve.
In the scheme, the method comprises the following steps: and cleaning oil stains on the surface of the 904L stainless steel plate by using alcohol.
In the scheme, the method comprises the following steps: in the step 4), a layer of powder with the thickness of 1-1.5mm is preset on the surface of the base material by using a stainless steel die.
In the scheme, the method comprises the following steps: the laser cladding parameters are that the laser power P is 2500W, the scanning speed v is 5mm/s, the rectangular light spot size is 20mm 2mm, and the air flow density is 15 L.min < -1 >.
The coating is prepared by the preparation method of the high-entropy alloy composite coating of the high-hardness nano TiC particle reinforced phosphoric acid reaction tank stirring paddle blade.
TiC is a chemically stable ceramic material with high melting point, high hardness and low density, and when the TiC is dispersed in a metal matrix in a granular manner, the TiC can be used as a hard point support in the sliding friction process of the material to improve the wear resistance, reduce the friction coefficient and play a good role in surface strengthening. Adding TiC into high-entropy alloy FeCoCrNi can introduce Ti and C atoms, and is beneficial to improving the performance of the high-entropy alloy. The high-entropy alloy contains a large amount of noble metal elements such as Co, Ni, Cr and the like, and the high-entropy alloy prepared by the traditional vacuum melting or casting method and the like needs a large amount of powder raw materials, so that the production cost is greatly increased. The surface coating technology of the invention can obviously improve the performance of the surface of the base material, reduce the consumption of high-entropy alloy and reduce the production cost. Compared with preparation methods such as plasma spraying, thermal spraying, chemical deposition, magnetron sputtering and the like, the laser cladding technology can obviously improve the performance of the metal substrate, and has the characteristics of rapid heating and cooling, small deformation, metallurgical bonding between the coating and the substrate, controllable coating thickness and the like. The FeCoCrNi + xvol% TiC composite component designed by the invention is used for preparing a high-entropy alloy composite coating on the surface of 904L stainless steel by a laser cladding technology, so that the high-entropy alloy component suitable for the environment conditions of strong acid corrosion and strong ore powder scouring is obtained, and a high-wear-resistant and corrosion-resistant material formula and a surface coating preparation technology are provided for the phosphorus chemical industry in China. The hardness, the wear resistance and the corrosion resistance of the high-entropy alloy are improved.
Drawings
Fig. 1 is a powder SEM morphology (a) CrFeCoNi (500x) (b) TiC ceramic particles (2000 x).
FIG. 2 is an XRD diagram of a FeCoCrNi + xvol% TiC composite high-entropy alloy coating.
FIG. 3 is a microstructure diagram of a FeCoCrNi + xvol% TiC composite high-entropy alloy coating.
Fig. 4 is a transmission topography of FeCoCrNi +5 vol% TiC, FeCoCrNi +12.5 vol% TiC composite coating, (a) 5TiC coating bright field phase (b) 5TiC coating selective diffraction spots (c)5TiC coating high resolution image and corresponding fourier transformation spots (d) EDS result of TiC particles in 5TiC coating (e)12.5 TiC coating bright field phase (f) f 12.5TiC coating selective diffraction spots.
FIG. 5 is an EBSD grain boundary map of FeCoCrNi +12.5 vol% TiC coating.
FIG. 6 is a hardness distribution diagram of FeCoCrNi + xvol% TiC composite high-entropy alloy.
FIG. 7 is a graph of the abrasion mass loss of the FeCoCrNi + xvol% TiC composite high-entropy alloy coating.
FIG. 8 is a friction and wear curve diagram of FeCoCrNi + xvol% TiC composite high entropy alloy.
FIG.9 is a wear scar morphology diagram of a FeCoCrNi + xvol% TiC composite high-entropy alloy coating.
FIG. 10 shows that the FeCoCrNi + xvol% TiC composite high-entropy alloy is at 0.5mol/L H2SO4Electrochemical profile in solution. (a) Polarization graph (b), impedance graph (c), modulus graph (d), phase angle graph.
Detailed Description
The present invention will be described in further detail below by way of specific embodiments:
example 1
1a) Designing components: taking FeCoCrNi high-entropy alloy as a matrix, and adding 5 vol%, 7.5 vol%, 10 vol%, 12.5 vol% and 15 vol% of nano TiC particles to obtain FeCoCrNi + xvol% TiC composite components (for convenience, the components are abbreviated as 5TiC, 7.5TiC, 10TiC, 12.5TiC and 15TiC), wherein specific chemical components are shown in Table I;
table chemical composition of high entropy alloy
(2) Powder selection: the FeCoCrNi high-entropy alloy powder is spherical powder with the size of 45-105 mu m and the purity of 99.0-99.5 percent, the TiC powder is irregular granular, the particle size is 5-15 mu m, the powder purity is more than or equal to 99.5 percent, and the powder morphology is shown in figure 1.
(3) The powder was prepared according to table one and weighed using an AL204 electronic balance with an accuracy of 0.1 mg.
(4) Powder ball milling: and (3) placing the prepared powder into a stainless steel ball milling tank for ball milling to uniformly mix the powder. The ball milling parameters are as follows: the ball material ratio is 5: 1, ball milling rotation speed of 250-. And (4) sieving the ball-milled powder by a 120-mesh stainless steel sample separating sieve, and placing the sample in vacuum drying for storage.
(5) Selecting a base material: 904L stainless steel plates with dimensions of 50mm (length) 30mm (width) 10mm (thickness) were selected as substrates, the substrate composition being listed in table two. Removing oxide skin on the cladding surface by using a handheld grinder, cleaning oil stain on the surface by using alcohol, drying by using a blower, drying, storing and the like.
Chemical composition of stainless Steel No. 904L (wt%)
(6) Preparing a laser cladding coating: a layer of powder with the thickness of 1.5mm is preset on the surface of a base material by a stainless steel die by adopting a powder prefabricating method, and is compacted by a stainless steel knife. Preparing a coating by adopting broadband laser cladding, introducing argon for protection in the cladding process, and specifically comprising the following parameters: the laser power P is 2500W, the scanning speed v is 5mm/s, the rectangular light spot size is 20mm 2mm, and the air flow density is 15 L.min-1。
FIG. 2 is an XRD pattern of a FeCoCrNi + xvol% TiC composite high-entropy alloy coating. From the XRD pattern of the FeCoCrNi + xvol% TiC composite high-entropy alloy coating in FIG. 2, it can be seen that the main phase of the composite coating is FCC solid solution, and when the addition of TiC exceeds 10 vol%, a weak TiC phase peak appears.
FIG. 3 is a microstructure diagram of a FeCoCrNi + xvol% TiC composite high-entropy alloy coating. (a) A FeCoCrNi coating and 904 base material combination area (b), a FeCoCrNi coating (c), a 5TiC coating (d), a 10TiC coating (d), a 7.5TiC coating (e), a 10TiC coating (f), a 12.5TiC coating (g), a 15TiC coating (h) and the TiC particle size (image J software statistics).
TiC content in table three FeCoCrNi + xvol% TiC composite high-entropy alloy coating structure (image J software statistics)
Fig. 3a shows the bonding area of the 0TiC coating and the substrate, where the coating and the substrate are in good metallurgical bonding, and at the bonding interface, a large amount of columnar crystals are generated perpendicular to the bonding interface due to the rapid heating and cooling of the laser. On top of the 0TiC coating (fig. 3b), the texture is a single equiaxed crystal. Fig. 3c-g shows the top structure of the xTiC (x ═ 5,7.5, 10,12.5) composite coating. With the addition of TiC, the grains of the coating are gradually refined. The average size of TiC particles in the 5TiC coating is about 0.46 mu m and is uniformly distributed among crystals. In a 7.5TiC coating (fig. 3d), most of the TiC particles are embedded in the matrix, except for a small amount of TiC precipitated along the grain boundaries. As TiC is added, the TiC particles coarsen in the 10TiC coating (fig. 3e) and are distributed along the grain boundaries. In a 12.5TiC coating (FIG. 3f), the average size of the precipitated TiC particles increases to 0.84 μm. In the 15TiC coating (fig. 3g), a large number of granular TiC particles are uniformly distributed on the substrate. And thirdly, counting the actual content of TiC precipitated particles in different TiC coatings. The actual content of precipitated particles of TiC in all coatings was slightly lower than the nominal content of the coating. Enthalpy of mixing is an important parameter for representing affinity between two elements, the lower the enthalpy of mixing between two elements, the more easily a stable compound is formed, and of the six elements of Fe, Co, Cr, Ni, Ti and C have the lowest enthalpy of mixing ((-109kJ/mol), so Ti and C are easily combined to form a TiC compound.
Fig. 4 is a transmission topography of FeCoCrNi +5 vol% TiC, FeCoCrNi +12.5 vol% TiC composite coating, (a) 5TiC coating bright field phase (b) 5TiC coating selective diffraction spots (c)5TiC coating high resolution image and corresponding fourier transformation spots (d) EDS result of TiC particles in 5TiC coating (e)12.5 TiC coating bright field phase (f) f 12.5TiC coating selective diffraction spots.
Fig. 4 shows the transmission morphology and corresponding diffraction spots of the 5TiC and 12.5TiC composite coatings, fig. 4a shows the bright field phase morphology of the coating, in-situ generation of off-white TiC particles, and good combination of the FCC substrate and TiC precipitation. TiC particles (0.2-0.6 μm) independently exist on the HEA substrate. In fig. 4a, the long TiC particles are mainly precipitated between grain boundaries, and the rectangular TiC particles are mainly precipitated inside the crystal grains. FIG. 4b selected diffraction spots of precipitated phases show that TiC particles have FCC edges
The ribbon axis is observed. TiC particle rim [011 in FIG. 4f]The ribbon axis is observed. Fig. 4c is a high resolution transmission image of the 5TiC coating and the corresponding fourier transformed spots, showing that the TiC/HEA interface is clear, no intermediate layer is formed, and the interface atoms are arranged in series, which is a semi-coherent interface. This has the advantage that the creation of an interface is beneficial for improving the performance of the composite coating.
FIG. 5 is an EBSD grain boundary map of FeCoCrNi +12.5 vol% TiC coating. It can be seen from the figure that fine TiC particles precipitate uniformly on the FCC substrate.
FIG. 6 is a hardness distribution diagram of a FeCoCrNi + xvol% TiC composite high-entropy alloy. It can be seen from the figure that the hardness of the coating is continuously improved with the addition of TiC, the 15TiC composite coating has the highest hardness, the average hardness reaches 357.4HV0.2 and is about 2 times of that of 904L stainless steel base material. However, the 15TiC composite coating has larger cross-sectional hardness fluctuation, which is probably caused by cracks generated in the preparation process of the coating due to high hardness of the coating.
FIG. 7 is a graph of the abrasion mass loss of the FeCoCrNi + xvol% TiC composite high-entropy alloy coating. As can be seen from the figure, the composite coating has a significantly lower loss of wear quality than the substrate, indicating that the composite coating has a higher wear resistance than the substrate. With the addition of TiC, the mass loss of the 0-12.5TiC coating gradually decreases, but the 15TiC wear increases slightly.
FIG. 8 is a friction and wear curve diagram of FeCoCrNi + xvol% TiC composite high entropy alloy. It can be seen from the figure that the wear curve initially increases sharply and then gradually stabilizes. As TiC is added, the average coefficient of friction of the coating gradually decreases, with the average coefficient of friction of the 12.5TiC coating being the lowest (fade 0.5803), but the average coefficient of friction of the 15TiC coating increases slightly, possibly due to the generation of cracks in the coating.
FIG.9 is a wear scar morphology diagram of a FeCoCrNi + xvol% TiC composite high-entropy alloy coating. From the figure it can be seen that in ab the substrate and the FeCoCrNi coating, a lot of flaking and oxidation phenomena occur due to the lower hardness. With the addition of TiC, the furrows of the composite coating become shallow gradually, and the spalling is reduced, which shows that the wear resistance is improved. A large number of discontinuous oxide layers and microcracks in the composite coating indicate adhesive and oxidative wear. The microcracks in the wear coating occur primarily because of the increased brittleness of the coating due to the precipitation of a large amount of TiC particles and the solid solution strengthening effect, which may cause brittle fracture under the action of friction side effects. The direction of the generation of the microcracks is random, which indicates that the failure appearance of the oxide layer on the worn surface is generated due to crack propagation.
FIG. 10 shows that the FeCoCrNi + xvol% TiC composite high-entropy alloy is at 0.5mol/L H2SO4Electrochemical profile in solution. (a) Polarization graph (b), impedance graph (c), modulus graph (d), phase angle graph.
The table of the four FeCoCrNi + xvol% TiC composite high-entropy alloy is 0.5mol/L H2SO4Electrochemical fitting parameters and impedance equivalent circuit fitting parameters in solution
FIG. 10a shows a composite coating andas can be seen from the substrate polarization curve, all samples were passivated in the anodic region and a passivation film was spontaneously formed. In general, the lower the corrosion current density, the higher the corrosion potential, indicating a better corrosion resistance of the material. The critical pitting potential indicates the ability of the passivation film to resist sustained breakdown of current. In combination with the relevant tafel fitting parameters in table four, the coating corrosion resistance gradually increased when the addition of TiC was below 12.5 vol%. The 12.5TiC coating has the highest corrosion potential (-410mV) and the smallest self-corrosion current density (0.1018 mA/cm)2) Indicating the best corrosion resistance. As TiC continues to increase, the corrosion potential of the coating decreases, the current density increases, and the corrosion resistance of the coating decreases. The 12.5TiC coating has the highest pitting potential (856.9mV) and smaller pitting current density (0.0577 mA/cm)2) Indicating a higher pitting resistance. A metastable pitting potential (Em) appeared in the 10-15 TiC coating, indicating breakdown of the passivation film. Local fluctuations can be ignored since they occur only in a small area. The TiC particles have thermodynamic stability and better electrochemical corrosion resistance, and can effectively improve the corrosion resistance of the composite coating. However, when the addition amount of TiC is too much, a large amount of TiC particles in a coating structure are precipitated, a microbattery is easily formed, the corrosion tendency is increased, and the corrosion resistance of the coating is reduced, so that when the addition amount of TiC is 12.5 vol%, the coating has better electrochemical corrosion resistance. Fig. 10b-d are the corresponding electrochemical impedance spectra, each sample impedance spectrum is a semi-circle, showing that the charge transfer controls the corrosion process, and the larger the semi-circle arc in the impedance plot is, the higher the interface transfer resistance is, the easier the passivation film is generated. The 12.5TiC coating has the largest radius of resistance followed by a 15TiC coating and the lowest by a FeCoCrNi coating. The impedance fitting parameters are shown in the fourth table, the polarization resistance Rp is gradually increased when x is less than or equal to 12.5, the Rp value is reduced when x is 15, and the Rp value of the 12.5TiC coating is maximum (2140 omega cm 2). In the mode value and phase angle diagram (FIG.9c-d), the impedance mode value | Z | represents the corrosion resistance of the material, and the larger | Z | is, the better the corrosion resistance is. The mode value | Z | stabilizes at a constant value in the high frequency region, while the phase angle value approaches 0, indicating that a coating with a resistance-like behavior occurs in the high frequency region. The impedance modulus | Z | curve slopes down in the low frequency region and the phase angle of each coating is greatest in the intermediate frequency region, indicating that the coatings have similar capacitancesAn action occurs. 12.5TiC has the largest phase angle (78 deg.), indicating an increase in corrosion resistance.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all of them should be covered in the claims of the present invention.
Claims (9)
1. A preparation method of a high-entropy alloy composite coating of high-hardness nano TiC particle reinforced phosphoric acid reaction tank stirring paddle blades is characterized by comprising the following steps:
1) accurately weighing FeCoCrNi high-entropy alloy powder and TiC particles;
2) placing FeCoCrNi high-entropy alloy powder and TiC particles into a ball milling tank for ball milling to ensure that the powder is uniformly mixed, and then sieving, drying and storing;
3) selecting a 904L stainless steel plate as a base material, removing surface oxide skin, cleaning surface oil stains, and drying for later use;
4) a layer of powder is preset on the surface of a base material by a stainless steel die by a powder prefabricating method, the base material is compacted by a stainless steel knife, a coating is prepared by broadband laser cladding, and argon is introduced for protection in the cladding process.
2. The preparation method of the high-hardness nano TiC particle reinforced phosphoric acid reaction tank stirring paddle blade high-entropy alloy composite coating according to claim 1, which is characterized by comprising the following steps: the addition amount of TiC is 5-12.5 vol%.
3. The preparation method of the high-hardness nano TiC particle reinforced phosphoric acid reaction tank stirring paddle blade high-entropy alloy composite coating according to claim 1 or 2, which is characterized by comprising the following steps: the FeCoCrNi high-entropy alloy powder is spherical powder with the size of 45-105 mu m and the purity of 99.0-99.5%, and the TiC powder is irregular particles with the particle size of 5-15 mu m and the powder purity of more than or equal to 99.5%.
4. The preparation method of the high-hardness nano TiC particle reinforced phosphoric acid reaction tank stirring paddle blade high-entropy alloy composite coating according to claim 3, which is characterized by comprising the following steps: the ball milling parameters are that the ball material ratio is 5: 1, ball milling rotation speed of 250-.
5. The preparation method of the high-hardness nano TiC particle reinforced phosphoric acid reaction tank stirring paddle blade high-entropy alloy composite coating according to claim 4, which is characterized by comprising the following steps: and sieving the ball-milled powder by a 120-mesh stainless steel sample sieve.
6. The preparation method of the high-hardness nano TiC particle reinforced phosphoric acid reaction tank stirring paddle blade high-entropy alloy composite coating according to claim 5, which is characterized by comprising the following steps: and cleaning oil stains on the surface of the 904L stainless steel plate by using alcohol.
7. The preparation method of the high-hardness nano TiC particle reinforced phosphoric acid reaction tank stirring paddle blade high-entropy alloy composite coating according to claim 6, which is characterized by comprising the following steps: in the step 4), a layer of powder with the thickness of 1-1.5mm is preset on the surface of the base material by using a stainless steel die.
8. The preparation method of the high-hardness nano TiC particle-reinforced phosphoric acid reaction tank stirring paddle blade high-entropy alloy composite coating according to claim 7, characterized by comprising the following steps: the laser cladding parameters are that the laser power P is 2500W, the scanning speed v is 5mm/s, the rectangular light spot size is 20mm 2mm, and the air flow density is 15 L.min < -1 >.
9. The coating prepared by the preparation method of the high-hardness nano TiC particle reinforced phosphoric acid reaction tank stirring paddle blade high-entropy alloy composite coating of any one of claims 1 to 8.
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