CN111014703A - Preparation method of nickel-based alloy powder for laser cladding - Google Patents
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- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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Abstract
The invention discloses a preparation method of nickel-based alloy powder for laser cladding, which comprises the following steps: step 1: putting the nickel-based alloy bar into a vacuum induction furnace for smelting to obtain a nickel-based alloy melt; step 2: pumping a smelting chamber, an atomizing chamber and a primary cyclone separator in a vacuum atomizing smelting furnace to a vacuum state, and filling argon for protection; and step 3: heating the nickel-based alloy melt to form nickel-based alloy melt, atomizing, and obtaining nickel-based alloy powder under the impact action of the ultrahigh-speed inert gas flow; and 4, step 4: screening and air-flowing the nickel-based alloy powder prepared in the step (3) according to the requirement of a laser cladding technology or a selective laser melting technology on the particle size of the powder; and 5: and (4) loading the nickel-based alloy powder obtained by screening and airflow in the step (4) into a vacuum degassing furnace, and carrying out vacuum degassing to finally obtain the nickel-based alloy powder with high sphericity. The method has the advantages that the prepared nickel-based alloy powder has high sphericity and high powder yield.
Description
Technical Field
The invention relates to the technical field of preparation methods of nickel-based alloy powder, in particular to a preparation method of nickel-based alloy powder for laser cladding.
Background
3D printing is a manufacturing technology that uses laser or electron beam and other means to add and pile up materials layer by layer under computer control to directly and rapidly form parts according to three-dimensional modeling, also called additive manufacturing. The additive manufacturing technology does not need traditional tools, clamps and a plurality of processing procedures, can quickly and accurately manufacture parts with any complex shapes on one device by utilizing three-dimensional design data, and has extremely high material utilization rate compared with the traditional processing of material removal (or deformation) and the common special processing technology.
Selective Laser Melting (SLM) is a method for directly forming metal parts, and is a latest development of metal additive manufacturing technology. The technology is based on the most basic idea of rapid forming, namely an incremental manufacturing mode of layer-by-layer cladding, parts with specific geometric shapes are directly formed according to a three-dimensional model, and metal powder is completely melted in the forming process to generate metallurgical bonding. The SLM can produce metal parts with complex shapes and structures which cannot be manufactured by the traditional machining means, greatly reduces machining procedures and shortens machining period. The metal powder materials currently used for SLM are titanium alloys, aluminum alloys, stainless steel, die steel, nickel-based alloys, etc.
Laser Cladding (Laser Cladding), also known as Laser Cladding or Laser Cladding, is a new surface modification technology. The method is a technological method which obviously changes the characteristics of the base material such as wear resistance, corrosion resistance, heat resistance and the like by adding cladding materials on the surface of the base material, presetting or synchronously feeding selected metal cladding materials on the surface of the base alloy, then melting the metal cladding materials and the surface layer of the base simultaneously through laser treatment, and rapidly solidifying the metal cladding materials into the surface layer which is in metallurgical bonding with the base material.
In industrial fields and civil metal materials, the proportion of the nickel-based alloy is large, the nickel-based alloy is one of the most important basic materials in the industry, and the added value of the nickel-based alloy is also large, particularly the nickel-based alloy. It has the following characteristics: (1) the product has good appearance glossiness; (2) the corrosion resistance is good, and especially the pitting corrosion resistance is excellent; (3) the high-temperature strength is excellent, and the processing hardenability and the creep resistance are excellent; (4) solid solution state is nonmagnetic. Nickel-base alloys combine properties, appearance and service characteristics, so it will remain one of the best industrial and domestic materials in the future. The nickel-based alloy parts manufactured by the traditional processes of casting, forging and the like respectively have the disadvantages of low macro-component segregation and material utilization rate, serious oxidation, irregular shape and unsatisfactory comprehensive performance after pressing, and the defects can be effectively overcome by adopting a 3D printing technology. The nickel-based alloy powder used for the 3D printing technology has powder characteristics different from those required for conventional powder metallurgy, and requires not only high powder purity and low oxygen content, but also high powder sphericity, uniform particle size distribution, and good fluidity and apparent bulk density.
At present, the main preparation method of metal powder is an air atomization method, the basic principle of which is the process of crushing liquid metal flow into small liquid drops by using high-speed airflow and quickly solidifying the small liquid metal drops into powder, and the powder prepared by the air atomization method has the advantages of high purity, low oxygen content, controllable powder granularity, low production cost, high sphericity and the like, can particularly meet the requirements of a 3D printing technology on the performance of the metal powder, and becomes the main development direction of the preparation technology of high-performance and special alloy powder.
Vacuum Induction Melting (VIM) is a metal process for melting metals under Vacuum by using the electromagnetic induction heating principle. Eddy current is generated during the electromagnetic induction heating process, so that the metal is melted. The process can be used to increase the purity of the alloy and reduce the oxygen content of the alloy.
The conventional method for improving and improving the fluidity of metal powder is to add a dispersant to reduce the friction between powder particles, thereby achieving the effect of improving the fluidity of the powder. However, the nickel-based alloy powder for laser cladding requires that the impurity content of the powder is very low, and more impurity elements are undoubtedly doped by adding the dispersing agent, so that the laser cladding forming is adversely affected.
The method for improving the sphericity of the powder particles in the powder atomization production is to increase the size of an atomization cylinder and improve the superheat degree of alloy droplets, but the increase of the size of the atomization cylinder and the superheat degree of the alloy can cause unstable production process and increase production cost, and is not beneficial to popularization and application of the 3D printing technology. .
Disclosure of Invention
The invention aims to provide a preparation method of nickel-based alloy powder for laser cladding.
The technical purpose of the invention is realized by the following technical scheme:
the preparation method of the nickel-based alloy powder for laser cladding is characterized by comprising the following steps of:
step 1: putting the nickel-based alloy bar into a vacuum induction furnace for smelting to obtain a nickel-based alloy melt;
step 2: pumping a smelting chamber, an atomizing chamber and a primary cyclone separator in a vacuum atomizing smelting furnace to a vacuum state, and filling argon as gas protection;
and step 3: heating the nickel-based alloy melt, controlling the superheat degree to reach 100-350 ℃, preserving the heat for 10 minutes after the nickel-based alloy melt is completely changed into the nickel-based alloy melt, pouring the nickel-based alloy melt into a tundish crucible, enabling the nickel-based alloy melt to flow into an atomizing chamber under the combined action of gravity and negative pressure suction force through a leak hole at the bottom of the tundish crucible, adjusting the atomizing pressure to be 4-6 MPa, crushing the nickel-based alloy melt into fine droplets under the impact action of ultrahigh-speed inert gas flow, cooling and solidifying the droplets to obtain nickel-based alloy powder, and bringing the nickel-based alloy powder into a powder collecting device of a primary cyclone separator by gas under the suction force of an air blower;
and 4, step 4: screening and air-flowing the nickel-based alloy powder prepared in the step (3) according to the requirement of a laser cladding technology or a selective laser melting technology on the particle size of the powder;
and 5: and (4) loading the nickel-based alloy powder obtained by screening and airflow in the step (4) into a vacuum degassing furnace, and carrying out vacuum degassing to finally obtain the nickel-based alloy powder with high sphericity.
Preferably, the nickel-based alloy bar material in the step 1 comprises the following raw material components in percentage by weight: 25-34% of Co, 26-30% of Cr, less than or equal to 1.5% of Fe, 1.85-2.95% of Si, 0.3-0.8% of Mn, 0.03-0.06% of C, less than or equal to 0.03% of S, less than or equal to 0.05% of P, and the balance of Ni.
Preferably, the pressure of the atomizing furnace pumped to the vacuum state in the step 2 is 7x10-3～9x10-3Pa。
Preferably, the temperature in the crucible of the tundish in the step 3 is controlled to be 900-1500 ℃.
Preferably, the inert gas in the step 3 is high-purity argon, and the atomization pressure in the atomization chamber is adjusted to be 4-6 MPa.
Preferably, the diameter of the leaking hole in the step 3 is 3-6 mm.
Preferably, the range of the particle size requirement of the nickel-based alloy powder by the selective laser melting technology in the step 4 is 15-45 μm; the range of the particle size requirement of the laser cladding technology on the nickel-based alloy powder is 45-180 mu m. .
Preferably, the powder loading height of each boat of the nickel-based alloy powder loaded in the step 4 is less than 14 mm.
Preferably, the vacuum degassing in step 4 is performed under the following conditions: 1.5X 10-2And (3) respectively preserving heat for 1-3 h at 200-550 ℃ and 550-700 ℃ in sequence under Pa vacuum.
In conclusion, the invention has the following beneficial effects:
1. the invention improves the fluidity of the 3D printing metal powder through a vacuum degassing process. The gas in the powder gap or surface is released in the vacuum degassing process. The vacuum degassing treatment can improve the flowability of the powder, because the smaller the particle size of the powder particles, the larger the surface energy is, the easier the gas is to be adsorbed, and the adsorbed gas can further promote the adhesion and agglomeration of the powder.
2. According to the method for preparing the nickel-based alloy powder by vacuum atomization, disclosed by the invention, as the vacuum atomization process is carried out in an inert atmosphere, the contact between an alloy liquid and oxygen is effectively isolated, and the oxidation of the powder is avoided, the oxygen content of the nickel-based alloy powder prepared by vacuum atomization is very low, the powder can be impacted by argon in the atomization process to achieve the effect of quenching, Cr forms a supersaturated solid solution in the molten liquid, Cr can be separated out in a fine particle form through subsequent heat treatment, the original fine grain structure of rapid solidification is kept, the strength of the alloy powder is improved, the proportion of spherical powder particles can be ensured to be more than 90%, and thus the prepared powder can be completely used for a 3D printing technology.
3. The preparation method has the advantages that different 3D printing technical characteristics are combined, the prepared powder is respectively used for different metal 3D printing technologies through vibration screening and airflow methods, the utilization rate of the powder is greatly improved, the problems that the utilization rate of the metal powder is too low and the metal powder is subjected to non-vacuum melting for conventional 3D printing are solved, the production cost is reduced, and obvious economic benefits are obtained.
4. The nickel-based alloy powder prepared by the invention has low impurity content, uniform particle size distribution, high powder particle sphericity which is more than or equal to 0.80, good powder fluidity (less than or equal to 17s/50g) and high apparent density (more than or equal to 4.5 g/cm)3) And the formed piece obtained by 3D printing has uniform and compact structure, high dimensional precision and excellent mechanical property.
Drawings
FIG. 1 is a particle morphology of the nickel-base alloy powder prepared in example 1;
FIG. 2 is a particle morphology of the nickel-based alloy powder prepared in example 2.
Detailed Description
The following further describes the embodiments of the present invention with reference to the drawings, and the present embodiment is not to be construed as limiting the invention.
Example 1:
the nickel-based alloy powder for the selective laser melting technique is prepared by the following steps:
(1) adding 250kg of nickel-based alloy bar raw material into a vacuum induction furnace for smelting to obtain a nickel-based alloy melt, wherein the nickel-based alloy bar raw material comprises the following components in percentage by weight: 45.78% of Ni, 25% of Co, 26% of Cr, 1.0% of Fe, 1.85% of Si, 0.3% of Mn, 0.03% of C, 0.01% of S and 0.03% of P.
(2) Pumping a smelting chamber, an atomizing chamber and a primary cyclone separator in a vacuum atomizing smelting furnace to a vacuum state with the vacuum degree of 7x10-3Pa, and filling argon as gas protection.
(3) Heating the nickel-based alloy melt, controlling the superheat degree to 150 ℃, keeping the temperature for 10 minutes after the nickel-based alloy melt is completely changed into the nickel-based alloy melt, simultaneously heating the tundish crucible to 900 ℃, enabling the nickel-based alloy melt to flow into the atomizing chamber through a leakage hole 3mm at the bottom of the tundish crucible under the combined action of gravity and negative pressure suction force, enabling the nickel-based alloy melt to be crushed into fine droplets under the impact action of high-purity argon flow, cooling and solidifying to obtain nickel-based alloy powder, enabling the nickel-based alloy powder to fall to the bottom of the atomizing cooling tower, and enabling the nickel-based alloy powder to be brought into a powder collecting device of a primary cyclone separator by gas under the suction force of a blower.
(4) And (4) screening and air-flowing the nickel-based alloy powder prepared in the step (3) according to the requirement of a selective laser melting technology on the particle size of the powder, wherein the particle size range is 15-45 mu m.
(5) Putting the nickel base alloy powder obtained by screening and airflow in the step (4) into a vacuum degassing furnace, wherein the powder loading height of each boat is less than 14mm, 5 boats are placed in each furnace, and the powder loading height is 1.5 multiplied by 10-2And (3) respectively preserving heat for 1h at 300 ℃ and 600 ℃ in Pa vacuum in sequence, and finally preparing the nickel-based alloy powder with high sphericity for the selective laser melting technology.
The particle morphology of the nickel-based alloy powder prepared by the embodiment is shown in figure 1, the average particle diameter is 37.87 mu m, the sphericity is 0.91, the fluidity is 14.7s/50g, and the apparent density is 3.88g/cm3The powder is subjected to SLM forming on EOS M280 equipment, the powder flowability is good in the powder laying process, the formed part is small in deformation and uniform in organization structure, and the mechanical property meets the use requirement of the part.
Example 2:
the nickel-based alloy powder for the laser cladding technology is prepared by the following steps:
(1) adding 250kg of nickel-based alloy raw materials into a vacuum induction furnace for smelting to obtain a nickel-based alloy melt, wherein the nickel-based alloy bar comprises the following raw materials in percentage by weight: 39.75% of Ni, 28% of Co, 28% of Cr, 1.2% of Fe, 2.45% of Si, 0.5% of Mn, 0.04% of C, 0.02% of S and 0.04% of P.
(2) Pumping a smelting chamber, an atomizing chamber and a primary cyclone separator in a vacuum atomizing smelting furnace to a vacuum state with the vacuum degree of 9x10-3Pa, and filling argon as gas protection.
(3) The nickel-based alloy melt is heated, the superheat degree is controlled to reach 200 ℃, after the nickel-based alloy melt is completely changed into the nickel-based alloy melt, the heat preservation is carried out for 10 minutes, meanwhile, the tundish crucible is heated to 1200 ℃, the nickel-based alloy melt flows into the atomizing chamber through a leakage hole 6mm at the bottom of the tundish crucible under the combined action of gravity and negative pressure suction force, the atomizing pressure in the gas atomizing furnace is 5MPa, the alloy melt is crushed into fine droplets under the impact action of high-purity argon flow, nickel-based alloy powder is obtained after cooling and solidification, the nickel-based alloy powder falls at the bottom of the atomizing cooling tower and is brought into a powder collecting device of a primary cyclone separator by gas under the suction force of a blower.
(4) And (4) screening and air-flowing the nickel-based alloy powder prepared in the step (3) according to the requirement of the laser cladding technology on the particle size of the powder, wherein the particle size range is 45-180 mu m.
(5) Putting the nickel base alloy powder obtained by screening and airflow in the step (4) into a vacuum degassing furnace, wherein the powder loading height of each boat is less than 14mm, 5 boats are placed in each furnace, and the powder loading height is 1.5 multiplied by 10-2Respectively keeping at 400 deg.C and 700 deg.C under Pa vacuumAnd (5) heating for 3h to finally prepare the nickel-based alloy powder with high sphericity for the laser cladding technology.
The particle morphology of the nickel-based alloy powder prepared by the embodiment is shown in figure 2, the average particle diameter is 103.5 mu m, the sphericity is 0.85, the fluidity is 20s/50g, and the apparent density is 4.75g/cm3The powder is subjected to laser cladding forming on a ZKZM-4000 device, the powder is uniformly spread and delivered, and the formed part has compact structure and small deformation.
Analysis of results
As shown in FIG. 1 and FIG. 2, the nickel-based alloy powder prepared by the present invention has no large amount of irregular powder particles, and it can be seen that the nickel-based alloy powder prepared by the present invention has the advantages of regular spherical microstructure, small amount of rod-like structure, dry powder, no obvious oxidation color particles, no visible inclusion, smooth surface, high sphericity and high powder yield.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes may be made and equivalents may be substituted without departing from the spirit and scope of the invention.
Claims (9)
1. The preparation method of the nickel-based alloy powder for laser cladding is characterized by comprising the following steps of:
step 1: putting the nickel-based alloy bar into a vacuum induction furnace for smelting to obtain a nickel-based alloy melt;
step 2: pumping a smelting chamber, an atomizing chamber and a primary cyclone separator in a vacuum atomizing smelting furnace to a vacuum state, and filling argon as gas protection;
and step 3: heating the nickel-based alloy melt, controlling the superheat degree to reach 100-350 ℃, preserving the heat for 10 minutes after the nickel-based alloy melt is completely changed into the nickel-based alloy melt, pouring the nickel-based alloy melt into a tundish crucible, enabling the nickel-based alloy melt to flow into an atomizing chamber under the combined action of gravity and negative pressure suction force through a leak hole at the bottom of the tundish crucible, adjusting the atomizing pressure to be 4-6 MPa, crushing the nickel-based alloy melt into fine droplets under the impact action of ultrahigh-speed inert gas flow, cooling and solidifying the droplets to obtain nickel-based alloy powder, and bringing the nickel-based alloy powder into a powder collecting device of a primary cyclone separator by gas under the suction force of an air blower;
and 4, step 4: screening and air-flowing the nickel-based alloy powder prepared in the step (3) according to the requirement of a laser cladding technology or a selective laser melting technology on the particle size of the powder;
and 5: and (4) loading the nickel-based alloy powder obtained by screening and airflow in the step (4) into a vacuum degassing furnace, and carrying out vacuum degassing to finally obtain the nickel-based alloy powder with high sphericity.
2. The method for preparing the nickel-based alloy powder for laser cladding according to claim 1, wherein the method comprises the following steps: the nickel-based alloy bar material in the step 1 comprises the following raw materials in percentage by weight: 25-34% of Co, 26-30% of Cr, less than or equal to 1.5% of Fe, 1.85-2.95% of Si, 0.3-0.8% of Mn, 0.03-0.06% of C, less than or equal to 0.03% of S, less than or equal to 0.05% of P, and the balance of Ni.
3. The method for preparing the nickel-based alloy powder for laser cladding according to claim 1, wherein the method comprises the following steps: the pressure of the atomization furnace pumped to the vacuum state in the step 2 is 7x10-3～9x10-3Pa。
4. The method for preparing the nickel-based alloy powder for laser cladding according to claim 1, wherein the method comprises the following steps: and in the step 3, the temperature in the tundish crucible is controlled to be 900-1500 ℃.
5. The method for preparing the nickel-based alloy powder for laser cladding according to claim 1, wherein the method comprises the following steps: and 3, the inert gas in the step 3 is high-purity argon, and the atomization pressure in the atomization chamber is adjusted to be 4-6 MPa.
6. The method for preparing the nickel-based alloy powder for laser cladding according to claim 1, wherein the method comprises the following steps: and in the step 3, the diameter of the leaking hole is 3-6 mm.
7. The method for preparing the nickel-based alloy powder for laser cladding according to claim 1, wherein the method comprises the following steps: the range of the requirement of the selective laser melting technology in the step 4 on the particle size of the nickel-based alloy powder is 15-45 mu m; the range of the particle size requirement of the laser cladding technology on the nickel-based alloy powder is 45-180 mu m.
8. The method for preparing the nickel-based alloy powder for laser cladding according to claim 1, wherein the method comprises the following steps: and in the step 4, the powder loading height of each boat of the nickel-based alloy powder loading boat is less than 14 mm.
9. The method for preparing the nickel-based alloy powder for laser cladding according to claim 1, wherein the method comprises the following steps: the vacuum degassing conditions in the step 4 are as follows: 1.5X 10-2And (3) respectively preserving heat for 1-3 h at 200-550 ℃ and 550-700 ℃ in sequence under Pa vacuum.
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| CN111549344A (en) * | 2020-06-29 | 2020-08-18 | 中天上材增材制造有限公司 | Nickel-based alloy powder for laser cladding |
| CN113369484A (en) * | 2021-06-08 | 2021-09-10 | 金川镍钴研究设计院有限责任公司 | Method for preparing low-oxygen-content vacuum gas atomization 3D printing high-temperature alloy powder |
| CN115283682A (en) * | 2022-08-26 | 2022-11-04 | 上海材料研究所 | Preparation method of nickel-based alloy powder with high tungsten content |
| CN115430838A (en) * | 2022-08-26 | 2022-12-06 | 上海材料研究所 | Preparation method of high-tungsten high-boron-content nickel-based alloy powder |
| CN115595471A (en) * | 2022-10-31 | 2023-01-13 | 湖南瑞华新材料有限公司（Cn） | Laser processing method for prolonging service life of conveying roller of continuous annealing furnace by using alloy powder |
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