CN114686872A - Strong corrosion-resistant Ta alloy coating and preparation method thereof - Google Patents
Strong corrosion-resistant Ta alloy coating and preparation method thereof Download PDFInfo
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- CN114686872A CN114686872A CN202210299019.5A CN202210299019A CN114686872A CN 114686872 A CN114686872 A CN 114686872A CN 202210299019 A CN202210299019 A CN 202210299019A CN 114686872 A CN114686872 A CN 114686872A
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- C—CHEMISTRY; METALLURGY
- C23—COATING 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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
- C23C24/082—Coating starting from inorganic powder by application of heat or pressure and heat without intermediate formation of a liquid in the layer
- C23C24/085—Coating with metallic material, i.e. metals or metal alloys, optionally comprising hard particles, e.g. oxides, carbides or nitrides
- C23C24/087—Coating with metal alloys or metal elements only
Abstract
A strong corrosion-resistant Ta/Nb composite coating and a preparation method thereof, the coating thickness is 5-35 μm, Ta + Nb is not less than 99 wt%, a solid embedding infiltration method is adopted; the raw material of the embedding agent is NH4Cl、Al2O3Ta and Nb powders. Compared with a spraying method, the temperature and the solidification process of the metal liquid drop in the spraying flying process are difficult to control accurately, so that a compact coating cannot be prepared, and meanwhile, the spraying method is difficult to be suitable for the surface of a curved surface or an inner cavity with small operation space. The embedding infiltration method is characterized in that the coating is formed by diffusing atoms, so that the coating can be completely compact theoretically, and the excellent performance of the coating under the strong corrosion-resistant working condition is ensured. The invention greatly reduces the reaction temperature, has simpler production equipment and process and high controllability of the thickness of the coating.
Description
Technical Field
The invention relates to a corrosion-resistant surface treatment method and a preparation technology thereof, in particular to a strong corrosion-resistant Ta alloy coating and a preparation method thereof.
Technical Field
In recent years, with the rapid development of economy in China, the number of various industrial devices is increasing, and the corrosion resistance problem is becoming more severe. The serious corrosion of metal in industrial production not only brings great hidden trouble to safety production, but also seriously affects the service life of equipment, and greatly affects the enterprise benefit and the social benefit.
At present, the preparation of corrosion-resistant coatings on the workpiece surfaces is recognized as the most effective protection method. The corrosion-resistant coating is usually prepared by methods such as spraying, but the coating prepared by the methods has weak bonding force with a metal workpiece, and certain holes are usually formed in the coating, so that the coating is easy to peel off in the using process, and the performance of the coating is difficult to meet the strong corrosion environment, such as a sulfuric acid pump. The development of a surface treatment method with strong binding force and excellent corrosion resistance is the key to prolonging the service life of the workpiece under the working conditions.
As an element with excellent corrosion resistance, Ta hardly reacts with various strong acids no matter under cold or hot conditions, and the surface layer is damaged by 0.006 mm only after being soaked in sulfuric acid at 200 ℃ for one year. The metal Nb is a refractory metal with a body-centered cubic structure, has good corrosion resistance, high melting point (2468 ℃), relatively low density (8.57 g/cm3), high-temperature strength, high thermal conductivity, small thermal neutron capture section, high superconducting critical temperature (9.2K), good weldability, ductility and excellent biocompatibility. The plasma spraying method commonly adopted for preparing the metal coating at present has low material utilization rate, easily causes a large amount of waste of metal powder in the spraying process and has high cost; in addition, certain pores inevitably exist in the metal coating prepared by plasma spraying, and a strong corrosive medium is easy to permeate into the surface of the matrix along the pores in the using process, so that the corrosion resistance of the coating is reduced.
Aiming at the defects of preparing the strong corrosion-resistant coating by a spraying method, the invention provides the strong corrosion-resistant Ta/Nb composite coating which is low in cost, high in efficiency, compact in prepared coating and simple in process and the preparation method thereof.
Disclosure of Invention
The invention provides a strong corrosion-resistant Ta alloy coating and a preparation method thereof. The base material is carbon steel or alloy steel, the thickness of the strong corrosion-resistant Ta alloy coating is 5-35 μm, the coating component is Ta or TaNb alloy, the content of Ta and Nb in the coating is not less than 99 wt%, and Ta is not less than 30 wt%, and the coating preparation method is a solid embedding infiltration method.
Further, the characterization method of the content of Ta and Nb elements in the coating comprises the following steps: weighing the mass of the workpiece before and after embedding, wherein the mass difference is used as the total mass of the coating, separating the total mass of the residual Ta + Nb powder after embedding by adopting a chemical filtration method, and the mass difference theory of Ta + Nb before and after embedding is used as the total mass of Ta + Nb in the coating; the characterization method of the Ta content in the coating is energy spectrum, line scanning is carried out in the coating thickness direction, the arithmetic mean content of Ta is calculated to serve as the Ta content in the coating, and the scanning line segment in the coating thickness direction is not less than 2.
The preparation method of the coating comprises the following steps:
(1) cleaning a workpiece, namely performing rust removal and oxidation removal treatment on the surface of the workpiece by adopting a mechanical method, and then degreasing and drying the workpiece;
(2) embedding agent proportioning: raw Material composition NH when preparing Ta coating4Cl、Al2O3Ta powder, NH when preparing Ta alloy coating4Cl、Al2O3Ta and Nb powders; wherein, the purity of Ta and Nb metal powder is not less than 99.9 wt%; the mass percentage ratio range of the four powders is Ta: nb: NH (NH)4Cl：Al2O30 for = 5 to 10 or 1 to 10 for = 1 to 10 and 70 to 89; the particle size of the metal powder is not less than 200 meshes, NH4Cl and Al2O3The content of the powder is not less than 99 wt%, and the granularity is not less than 100 meshes; mechanically mixing the four kinds of powder according to the proportion;
further, when preparing the Ta coating, the Nb powder proportion is 0, and when preparing the Ta alloy coating, the Nb powder proportion is selected to be 5-10;
(3) placing a workpiece into a crucible made of heat-resistant metal, covering the workpiece with the embedding agent, and placing the workpiece in a vacuum furnace, wherein the thickness of the embedding agent required for preparing the strong corrosion-resistant composite coating is not less than 2 mm, the crucible is sealed mechanically, and a sealing medium adopts glass; vacuum degree lower than 10-2After Pa, argon with the purity of 99.99 percent is introduced, and the pressure in the furnace is kept to be 1 +/-0.1 multiplied by 105Pa, the heating rate of the vacuum furnace is 5-10 ℃/min, the embedding infiltration temperature is 800-1200 ℃, and the embedding infiltration time is 5-30 h;
furthermore, the crucible is divided into a crucible cylinder and a crucible cover, a sealing groove is formed in the end face of the crucible cylinder, which is in contact with the crucible cover, glass is placed in the sealing groove in advance, and then the two parts of the crucible are connected by interference fit or bolts, so that sealing of the molten glass is realized;
(4) cleaning the workpiece, ultrasonic cleaning with water solution, and air drying.
The invention has the advantages that:
1. compared with a spraying method, the tantalum melting point is close to 3000 ℃, and the tantalum alloy coating is difficult to prepare by flame spraying, so that the tantalum alloy coating can only adopt a high-energy spraying method such as plasma, the reaction temperature is greatly reduced, the production equipment is simpler, and the process controllability is higher;
2. especially in the preparation of the coating with the complicated special-shaped curved surface such as narrow slit, the coating thickness is difficult to control or even cannot be prepared by a spraying method, the embedding infiltration method can be perfectly suitable for the preparation of various complicated curved surface coatings, and the thickness of the strong corrosion-resistant coating is controllable between 5 and 35 mu m by adjusting the embedding temperature and time;
3. compared with the spraying method, the method is suitable for various inner surface treatments, and particularly can solve the problem of preparation of inner cavity surface coatings on the inner wall of a pipe and without operation space of the spraying method;
4. the sealing of the crucible is realized by adopting the molten glass, and a certain amount of gas leakage exists on the sealing surface of the crucible before the glass is molten, so that the problem of gas discharge in the crucible during the vacuum pumping can be perfectly solved, the influence of oxygen is eliminated, and the difficulty in designing and manufacturing the sealing structure of the crucible is reduced;
5. compared with a spraying method, the temperature of the metal liquid is difficult to accurately control in the flying process, so that the coating cannot be used for preparing a compact coating, and the coating is formed by diffusing atoms in an embedding infiltration method, so that the coating can be completely compact theoretically, and the excellent performance of the coating under the strong corrosion-resistant working condition is ensured.
Drawings
FIG. 1 is an SEM photograph of a Ta alloy coating prepared in example 1, (1) the base material, 45 steel; (2) the coating is a Ta alloy coating, the content of Ta and Nb in the coating is not less than 99 percent by weight, the content of Ta element is not less than 42 +/-3 percent by weight, and the thickness of the coating is 12 +/-2 mu m.
FIG. 2 is a comparison of polarization curves for Ta alloy and 45 steel, where (1) the polarization curve for alloy coatings prepared in example 2, (2) the polarization curve for 45 steel, and (3) the polarization curve for coatings prepared in example 1. 45 steel and concreteThe corrosion potentials of the embodiment 2 and the embodiment 1 are-0.4434V, -0.12315V and-0.05985V respectively, and the corrosion current densities are as follows: 5.3X 10-3A/cm2 2.2×10- 7A/cm2 3.1×10-7A/cm2The corrosion potential of the embedded and infiltrated Ta alloy coating is improved by 7-8 times compared with that of the base material, and the corrosion current is reduced by about 104And (4) doubling.
Detailed Description
Example 1
A strong corrosion-resistant Ta/Nb composite coating and a preparation method thereof. The base material is 45 steel, the thickness of the strong corrosion-resistant Ta alloy coating is 12 +/-2 mu m, the content of Ta + Nb in the coating is not less than 99 percent by weight, and the content of Ta in the coating is not less than 42 +/-3 percent by weight, and the preparation method of the coating is a solid embedding infiltration method.
The preparation method of the coating comprises the following steps:
(1) cleaning a workpiece, namely performing rust removal and oxidation removal treatment on the surface of the workpiece by adopting a mechanical method, and then degreasing and drying the workpiece;
(2) the embedding agent is prepared by the following steps: the raw material is NH4Cl、Al2O3Ta and Nb powder, wherein the purity of the Ta and Nb metal powder is not less than 99.9 wt%; the four powders are Ta: nb: NH4Cl：Al2O3= 8: 6: 7: 79; the particle size of the metal powder is not less than 200 meshes, NH4Cl and Al2O3The granularity of the powder is not less than 100 meshes; mechanically mixing the powder for 1h according to the proportion;
(3) covering the workpiece with the embedding agent, and then placing the workpiece in a vacuum furnace, wherein the thickness of the embedding agent required for preparing the strong corrosion-resistant composite coating is not less than 3 mm; vacuum degree lower than 10-2After Pa, argon with the purity of 99.99 percent is introduced, and the pressure in the furnace is kept to be 1 +/-0.1 multiplied by 105Pa, the heating rate of the vacuum furnace is 5-10 ℃/min, the embedding infiltration temperature is 1000 +/-20 ℃, and the embedding infiltration time is 8 h;
(4) and cleaning the workpiece, and ultrasonically cleaning and air-drying by adopting an aqueous solution.
Example 2
A strong corrosion-resistant Ta alloy coating and a preparation method thereof. The base material is 45 steel, the thickness of the strong corrosion-resistant Ta alloy coating is 8 +/-2 mu m, the content of Ta + Nb in the coating is not less than 99 wt%, and the content of Ta is not less than 40 +/-3 wt%, and the coating preparation method is a solid embedding infiltration method.
The preparation method of the coating comprises the following steps:
(1) cleaning a workpiece, namely performing rust removal and oxidation removal treatment on the surface of the workpiece by adopting a mechanical method, and then degreasing and drying the workpiece;
(2) embedding agent proportioning: the raw material is NH4Cl、Al2O3Ta and Nb powder, wherein the purity of the Ta and Nb metal powder is not less than 99.9 wt%; the four powders are Ta: nb: NH (NH)4Cl：Al2O3= 8: 8: 7: 77; the particle size of the metal powder is not less than 200 meshes, NH4Cl and Al2O3The granularity of the powder is not less than 100 meshes; mechanically mixing the powder for 1h according to the proportion;
(3) covering the workpiece with the embedding agent, and then placing the workpiece in a vacuum furnace, wherein the thickness of the embedding agent required for preparing the strong corrosion-resistant composite coating is not less than 3 mm; vacuum degree lower than 10-2After Pa, argon with the purity of 99.99 percent is introduced, and the pressure in the furnace is kept to be 1 +/-0.1 multiplied by 105Pa, the heating rate of the vacuum furnace is 5-10 ℃/min, the embedding infiltration temperature is 900 +/-20 ℃, and the embedding infiltration time is 5 h;
(4) and cleaning the workpiece, and ultrasonically cleaning and air-drying by adopting an aqueous solution.
Claims (5)
1. A strong corrosion-resistant Ta alloy coating and a preparation method thereof are characterized in that a matrix material is carbon steel or alloy steel, the thickness of the strong corrosion-resistant Ta alloy coating is 5-35 mu m, the coating component is Ta or TaNb alloy, the content of Ta and Nb in the coating is not less than 99 wt%, and the content of Ta is not less than 30 wt%, and the preparation method of the coating is a solid embedding infiltration method; the preparation of the coating comprises the following steps:
(1) cleaning a workpiece, namely performing rust removal and oxidation removal treatment on the surface of the workpiece by adopting a mechanical method, and then degreasing and drying the workpiece;
(2) the embedding agent is prepared by the following steps: NH as starting material when preparing Ta coatings4Cl、Al2O3Ta powder, NH if preparing Ta alloy coating4Cl、Al2O3Ta and NbPowder; wherein, the purity of Ta and Nb metal powder is not less than 99.9 wt%; the particle size of the metal powder is not less than 200 meshes, NH4Cl and Al2O3The content of the powder is not less than 99 wt%, and the granularity is not less than 100 meshes; mechanically mixing the four kinds of powder according to the proportion;
further, when preparing the Ta coating, the Nb powder proportion is 0, and when preparing the Ta alloy coating, the Nb powder proportion is 0-5;
(3) covering the workpiece with the embedding agent, and then placing the workpiece in a vacuum furnace, wherein the embedding infiltration temperature is 800-1200 ℃, and the embedding infiltration time is 5-30 h;
(4) and cleaning the workpiece, and ultrasonically cleaning and air-drying by adopting an aqueous solution.
2. A strong corrosion-resistant Ta alloy coating is characterized in that the characterization method of the coating components comprises the following steps: weighing the mass of the workpiece before and after embedding, wherein the mass difference is used as the total mass of the coating, separating the total mass of the residual Ta + Nb powder after embedding by adopting a chemical filtration method, and the mass difference theory of Ta + Nb before and after embedding is used as the total mass of Ta + Nb in the coating; the characterization method of the Ta content in the coating is energy spectrum, line scanning is carried out in the coating thickness direction, the arithmetic mean content of Ta is calculated to serve as the Ta content in the coating, and the scanning line segment in the coating thickness direction is not less than 2.
3. The method for preparing a Ta alloy coating with strong corrosion resistance as claimed in claim 1, wherein the four powders are prepared from Ta: nb: NH (NH)4Cl：Al2O3= 5 to 10: 0 or (5-10): (1-10): (70 to 89);
further, when the Ta coating is prepared, the Nb powder ratio is 0, and if the Ta alloy coating is prepared, the Nb powder ratio is selected to be 5-10.
4. The method as claimed in claim 1, wherein the surface of the Ta alloy coating for making a strong corrosion-resistant coating on the workpiece is covered with a burying agent, and the thickness of the Ta alloy coating is not less than 2 mm; the vacuum degree in the furnace is less than 10-2After Pa, the purity is introduced99.99% argon gas, the pressure in the furnace is kept at 1 +/-0.1 x 105Pa, and the heating rate of the vacuum furnace is 5-10 ℃/min.
5. The method as claimed in claim 1, wherein the crucible is made of heat-resistant metal, the crucible is mechanically sealed, and the sealing medium is glass;
furthermore, the crucible is divided into a crucible cylinder and a crucible cover, a sealing groove is formed in the end face of the crucible cylinder, which is in contact with the crucible cover, glass is placed in the sealing groove in advance, and then the two parts of the crucible are connected through interference fit or bolts, so that sealing of the molten glass is realized.
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