CN112045195B - Metal powder for 3D printing and metal powder surface nano modification method - Google Patents
Metal powder for 3D printing and metal powder surface nano modification method Download PDFInfo
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/142—Thermal or thermo-mechanical treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B33Y70/00—Materials specially adapted for additive manufacturing
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- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/04—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling
- B22F2009/043—Making metallic powder or suspensions thereof using physical processes starting from solid material, e.g. by crushing, grinding or milling by ball milling
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Abstract
The invention discloses metal powder for 3D printing and a metal powder surface nano modification method. The nano modification method for the metal powder surface comprises the following steps: adding a metal powder raw material into a ball mill, vacuumizing the ball mill to a vacuum degree of not higher than 0.01Pa, introducing inert gas into the ball mill, heating to 100-500 ℃, preserving heat for 1-5 h, naturally cooling, and screening the cooled material to obtain a finished product. The method is simple and controllable, nano modification treatment can effectively reduce metal powder agglomeration, promote the physical state of the surface of the metal powder, and improve the fluidity of the powder; the metal powder for 3D printing obtained by the method is spherical or nearly spherical, has excellent fluidity and high apparent density, does not increase oxygen content and impurity content compared with the metal powder raw material, and can meet the requirement of 3D printing on the metal powder.
Description
Technical Field
The invention relates to the technical field of 3D printing, in particular to metal powder for 3D printing and a metal powder surface nano modification method.
Background
The 3D printing is used as a processing technology breaking through the traditional preparation technology, is an emerging manufacturing technology for manufacturing solid objects by stacking materials layer by layer based on a digital model, is suitable for design research, development, verification and the like before the production of complex micro-component products, personalized customization and large-scale production, has the advantages of high production efficiency, high material utilization rate, no need of a die and the like, and is a popular topic in the wind gap wave tip internationally at present.
The existing metal powder preparation technology for 3D printing mainly comprises the following steps: mechanical disruption, atomization, PREP, chemical methods, and the like; the mechanical crushing method is suitable for brittle materials, and the prepared powder has poor sphericity; the powder prepared by the PREP method has thicker granularity and higher cost; the chemical method has higher cost and is easy to introduce toxic and harmful impurities; the atomization method is a main method for preparing the metal powder for 3D printing at present, and the metal powder prepared by the aerosol method has good sphericity and reasonable granularity, but has the problems of poor fluidity of the satellite balls and the powder.
Therefore, it is necessary to further modify the metal powder produced by the aerosol method to have both low impurity content and good surface physical state.
Disclosure of Invention
The invention aims to provide metal powder for 3D printing and a metal powder surface nano modification method so as to solve the technical problems.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
in a first aspect, the invention provides a metal powder surface nano modification method, which comprises the following steps:
adding a metal powder raw material into a ball mill, vacuumizing the ball mill to a vacuum degree of not higher than 0.01Pa, introducing inert gas into the ball mill, heating to 100-500 ℃, preserving heat for 1-5 h, naturally cooling, and screening the cooled material to obtain a finished product.
Preferably, the metal powder raw materials are alloy powder subjected to gas atomization treatment and simple substance metal powder subjected to gas atomization treatment.
Further preferably, the alloy powder is selected from one or more of nickel-based alloy powder, aluminum-based alloy powder, cobalt-based alloy powder, stainless steel powder, die steel alloy powder.
Preferably, the particle size of the metal powder feedstock is no greater than 150 μm.
Preferably, the inert gas is selected from one or more of nitrogen, argon and helium.
Further preferably, the inert gas is argon.
Preferably, the air pressure of the ball mill is 1.0x10 after the inert gas is introduced 5 ～1.5×10 5 Pa。
Preferably, the step of screening the cooled material specifically includes: firstly removing the material with the granularity smaller than 15 mu m, and then selecting the material with the granularity smaller than 53 mu m.
Preferably, the finished product is spherical or nearly spherical in shape.
In a second aspect, the present invention provides a metal powder for 3D printing, which is prepared by using the metal powder surface nano modification method in the first aspect.
Compared with the prior art, the invention has the beneficial effects that:
the metal powder surface nano modification method provided by the invention has the advantages of simplicity and controllability, and under the action of inert gas, the nano layer grows in situ on the metal powder surface in the high-temperature treatment process to modify the metal powder surface, so that the agglomeration of the metal powder is effectively reduced, the physical state of the metal powder surface is improved, and the fluidity of the powder is improved; the metal powder for 3D printing obtained by the method is spherical or nearly spherical, has excellent fluidity and high apparent density, does not increase oxygen content and impurity content compared with the metal powder raw material, and can meet the requirement of 3D printing on the metal powder.
Drawings
FIG. 1 is an electron microscopic view of the nano-modified nickel-based alloy powder provided in example 1 of the present invention.
Detailed Description
The following describes the invention in more detail. The description of these embodiments is provided to assist understanding of the present invention, but is not intended to limit the present invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
In a first aspect, the invention provides a metal powder surface nano modification method, which comprises the following steps:
adding a metal powder raw material into a ball mill, vacuumizing the ball mill to a vacuum degree of not higher than 0.01Pa, introducing inert gas into the ball mill, heating to 100-500 ℃, preserving heat for 1-5 h, naturally cooling, and screening the cooled material to obtain a finished product.
It is understood that the nano modification can be fully completed on the surface of the metal powder under specific heat treatment conditions, so that the fluidity of powder particles is improved, the agglomeration of the metal powder is avoided, the heat treatment temperature is not more than 500 ℃, and the oxidation of the metal powder can be caused due to the excessive temperature, so that the impurity content is increased.
In one embodiment, the metal powder raw material is an alloy powder subjected to gas atomization treatment and an elemental metal powder subjected to gas atomization treatment.
Further, the alloy powder is selected from one or more of nickel-based alloy powder, aluminum-based alloy powder, cobalt-based alloy powder, stainless steel powder and die steel alloy powder.
In one embodiment, the metal powder feedstock has a particle size of no greater than 50 μm, which is advantageous in improving the processing efficiency of the metal powder feedstock.
In one embodiment, the inert gas is selected from one or more of nitrogen, argon, helium.
Further, the inert gas is argon.
In one embodiment, the ball mill is inflated with inert gas at a pressure of 1.0X10 5 ～1.5×10 5 Too high pressure Pa requires too high equipment and too low pressure tends to cause air ingress, which in turn contaminates the powder.
In one embodiment, the step of screening the cooled material specifically includes: firstly removing the material with the granularity smaller than 15 mu m, and then selecting the material with the granularity smaller than 53 mu m. The screening efficiency of the powder can be effectively improved on the premise of ensuring the granularity of the target product through grading screening, so that the powder has a good screening effect.
In one embodiment, the finished product is spherical or nearly spherical in shape, has excellent flowability and high apparent density, does not increase oxygen content and impurity content compared with the metal powder raw material, and can meet the requirement of 3D printing on metal powder.
In a second aspect, the present invention provides a metal powder for 3D printing, which is prepared by using the metal powder surface nano modification method in the first aspect.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
Adding nickel base alloy powder (particle size less than or equal to 150 μm) into a ball mill, vacuumizing the ball mill to vacuum degree of 0.01Pa, and introducing argon gas into the ball mill to maintain air pressure in the ball mill at 1.0X10% 5 Pa, heating to 220 ℃, preserving heat for 2.5h, then naturally cooling, adding the cooled material into a classifying screening machine, firstly removing the material with the granularity smaller than 15 mu m, and then screening the material with the granularity smaller than 53 mu m to obtain the nano modified nickel-based alloy powder with the granularity of 15-53 mu m.
The electron microscopic image of the finished product obtained in this example was tested, the results are shown in fig. 1, and the impurity content, particle size distribution and flowability of the nano-modified nickel-base alloy powder and the nickel-base alloy powder raw material after the gas atomization treatment were tested, and the test results are shown in table 1.
TABLE 1 results of testing impurity content, particle size distribution and flowability before and after modification of metal powder
As can be seen from the test results of fig. 1, the nano modified nickel-based alloy powder prepared in this example is spherical or nearly spherical; as shown by the test results in Table 1, compared with the raw material of the nickel-base alloy powder after the gas atomization treatment, the nickel-base alloy powder has excellent fluidity and high apparent density, the impurity content of the powder after the nano modification treatment is not changed obviously, the nano modification treatment does not increase the impurity (oxygen and nitrogen) content, and the results show that the nano modified nickel-base alloy powder prepared by the embodiment can meet the requirement of 3D printing on metal powder.
Example 2
Adding the cobalt-base alloy powder (granularity is less than or equal to 150 μm) subjected to gas atomization treatment into a ball mill, vacuumizing the ball mill to the vacuum degree of 0.008Pa, and introducing argon into the ball mill to keep the air pressure in the ball mill at 1.1X10 × 5 Pa, heating to 250 ℃, preserving heat for 3.0h, then naturally cooling, adding the cooled material into a classifying screening machine, firstly removing the material with the granularity smaller than 15 mu m, and then screening the material with the granularity smaller than 53 mu m to obtain the nano modified cobalt-base alloy powder with the granularity of 15-53 mu m.
As can be seen by electron microscope observation, the nano modified cobalt-based alloy powder prepared by the embodiment is spherical or nearly spherical.
The impurity content, particle size distribution and flowability of the nano modified cobalt-base alloy powder and the cobalt-base alloy powder raw material after the gas atomization treatment were tested, and the test results are shown in table 2.
TABLE 2 results of measurements of impurity content, particle size distribution and flowability before and after modification of metal powder
As shown by the test results in Table 2, compared with the raw material of the cobalt-base alloy powder after the gas atomization treatment, the cobalt-base alloy powder has excellent fluidity and high apparent density, the impurity content of the cobalt-base alloy powder after the nano modification treatment is not obviously changed, the nano modification treatment does not increase the impurity (oxygen and nitrogen) content, and the results show that the nano modified cobalt-base alloy powder prepared by the embodiment can meet the requirement of 3D printing on metal powder.
Example 3
Adding the die steel alloy powder (granularity is less than or equal to 150 μm) subjected to gas atomization treatment into a ball mill, vacuumizing the ball mill to the vacuum degree of 0.009Pa, and introducing argon gas into the ball mill to keep the air pressure in the ball mill at 1.0 multiplied by 10 5 Pa, heating to 210 ℃, preserving heat for 2.0h, then naturally cooling, adding the cooled material into a classifying screening machine, firstly removing the material with the granularity smaller than 15 mu m, and then screening the material with the granularity smaller than 53 mu m to obtain the nano modified die steel alloy powder with the granularity of 15-53 mu m.
As can be seen by electron microscope observation, the nano modified die steel alloy powder prepared by the embodiment is spherical or nearly spherical.
The nano modified die steel alloy powder and the die steel alloy powder raw material after the gas atomization treatment were tested for impurity content, particle size distribution and flowability, and the test results are shown in table 3.
TABLE 3 results of measurements of impurity content, particle size distribution and flowability before and after modification of metal powder
As can be seen from the test results in table 3, compared with the die steel alloy powder raw material after the gas atomization treatment, the die steel alloy powder has excellent fluidity and high apparent density, the impurity content of the die steel alloy powder after the nano modification treatment is not obviously changed, the nano modification treatment does not increase the impurity (oxygen and nitrogen) content, and the above results indicate that the nano modified die steel alloy powder prepared in the embodiment can meet the requirement of 3D printing on metal powder.
Example 4
Adding the aluminum alloy powder (granularity is less than or equal to 150 μm) subjected to gas atomization treatment into a ball mill, vacuumizing the ball mill to the vacuum degree of 0.009Pa, and introducing argon gas into the ball mill to keep the air pressure in the ball mill at 1.1X10 × 5 Pa, heating to 150 ℃, preserving heat for 2.5h, then naturally cooling, adding the cooled material into a classifying screening machine, firstly removing the material with the granularity smaller than 15 mu m, and then screening the material with the granularity smaller than 53 mu m to obtain the nano modified aluminum alloy powder with the granularity of 15-53 mu m.
As can be seen by electron microscope observation, the nano modified aluminum alloy powder prepared by the embodiment is spherical or nearly spherical.
The impurity content, particle size distribution and flowability of the nano-modified aluminum alloy powder and the aluminum alloy powder raw material after the gas atomization treatment were tested, and the test results are shown in table 4.
TABLE 4 results of tests for impurity content, particle size distribution and flowability before and after modification of metal powder
As can be seen from the test results in table 4, compared with the raw material of the aluminum alloy powder after the gas atomization treatment, the aluminum alloy powder has excellent fluidity and high bulk density, the impurity content of the aluminum alloy powder after the nano modification treatment is not changed significantly, the nano modification treatment does not increase the impurity (oxygen and nitrogen) content, and the above results indicate that the nano modified aluminum alloy powder prepared in this example can meet the requirements of 3D printing on the metal powder.
Example 5
Adding the stainless steel powder (particle size less than or equal to 150 μm) subjected to gas atomization treatment into a ball mill, vacuumizing the ball mill to a vacuum degree of 0.01Pa, and introducing argon gas into the ball mill to maintain the gas pressure in the ball mill to be 1.1X10% 5 Pa, heating to 200deg.C, maintaining the temperature for 2.5h, naturally cooling, adding the cooled materialAnd (3) putting the mixture into a classifying and screening machine, firstly removing materials with the granularity smaller than 15 mu m, and then screening out materials with the granularity smaller than 53 mu m to obtain the nano modified stainless steel powder with the granularity of 15-53 mu m.
As can be seen by electron microscopy, the nano modified stainless steel powder prepared in the embodiment is spherical or nearly spherical.
The nano-modified stainless steel powder and the stainless steel powder raw material after the gas atomization treatment were tested for impurity content, particle size distribution and flowability, and the test results are shown in table 5.
TABLE 5 test results of impurity content, particle size distribution and flowability before and after modification of metal powder
As can be seen from the test results in table 5, compared with the stainless steel powder raw material after the gas atomization treatment, the nano modified stainless steel powder has excellent fluidity and high bulk density, the impurity content of the stainless steel powder after the nano modification treatment is not changed significantly, the nano modification treatment does not increase the impurity (oxygen and nitrogen) content, and the above results indicate that the nano modified stainless steel powder prepared in this example can meet the requirement of 3D printing on metal powder.
Example 6
Adding nickel-base alloy powder (with granularity less than or equal to 150 mu m) subjected to gas atomization treatment into a ball mill, vacuumizing the ball mill to the vacuum degree of 0.01Pa, introducing argon into the ball mill, keeping the air pressure in the ball mill at 1.5 multiplied by 105Pa, heating to 100 ℃, preserving heat for 5.0h, naturally cooling, adding the cooled material into a classifying screening machine, firstly removing the material with granularity less than 15 mu m, and then screening the material with granularity less than 53 mu m to obtain the nano modified nickel-base alloy powder with granularity of 15-53 mu m.
As can be seen by electron microscope observation, the nano modified nickel-based alloy powder prepared by the embodiment is spherical or nearly spherical.
The nano modified nickel-based alloy powder and the nickel-based alloy powder raw material after the gas atomization treatment were tested for impurity content, particle size distribution and fluidity, and the test results are shown in Table 6
TABLE 6 test results of impurity content, particle size distribution and flowability before and after modification of metal powder
Example 7
Adding nickel base alloy powder (particle size less than or equal to 150 μm) into a ball mill, vacuumizing the ball mill to vacuum degree of 0.01Pa, and introducing argon gas into the ball mill to maintain air pressure in the ball mill at 1.0X10% 5 Pa, heating to 500 ℃, preserving heat for 1.0h, then naturally cooling, adding the cooled material into a classifying screening machine, firstly removing the material with the granularity smaller than 15 mu m, and then screening the material with the granularity smaller than 53 mu m to obtain the nano modified nickel-based alloy powder with the granularity of 15-53 mu m.
As can be seen by electron microscope observation, the nano modified nickel-based alloy powder prepared by the embodiment is spherical or nearly spherical.
The nano modified nickel-based alloy powder and the nickel-based alloy powder raw material after the gas atomization treatment were tested for impurity content, particle size distribution and fluidity, and the test results are shown in Table 7
TABLE 7 test results of impurity content, particle size distribution and flowability before and after modification of metal powder
Example 8
Adding nickel base alloy powder (particle size less than or equal to 150 μm) into a ball mill, vacuumizing the ball mill to vacuum degree of 0.01Pa, and introducing nitrogen gas into the ball mill to maintain the air pressure in the ball mill at 1.0X10% 5 Pa, heating to 220 ℃ and keepingAnd (3) heating for 2.5h, naturally cooling, adding the cooled material into a classifying screening machine, firstly removing the material with the granularity smaller than 15 mu m, and then screening the material with the granularity smaller than 53 mu m to obtain the nano modified nickel-based alloy powder with the granularity of 15-53 mu m.
As can be seen by electron microscope observation, the nano modified nickel-based alloy powder prepared by the embodiment is spherical or nearly spherical.
The impurity content, particle size distribution and fluidity of the nano modified nickel-based alloy powder and the nickel-based alloy powder raw material after the gas atomization treatment were tested, and the test results are shown in Table 8
TABLE 8 results of tests for impurity content, particle size distribution and flowability before and after modification of metal powder
Example 9
Adding nickel base alloy powder (particle size less than or equal to 150 μm) into a ball mill, vacuumizing the ball mill to vacuum degree of 0.01Pa, and introducing argon gas into the ball mill to maintain air pressure in the ball mill at 1.0X10% 5 Pa, heating to 600 ℃, preserving heat for 2.5h, then naturally cooling, adding the cooled material into a classifying screening machine, firstly removing the material with the granularity smaller than 15 mu m, and then screening the material with the granularity smaller than 53 mu m to obtain the nano modified nickel-based alloy powder with the granularity of 15-53 mu m.
As can be seen by electron microscope observation, the nano modified nickel-based alloy powder prepared by the embodiment is spherical or nearly spherical.
The nano modified nickel-based alloy powder and the nickel-based alloy powder raw material after the gas atomization treatment were tested for impurity content, particle size distribution and fluidity, and the test results are shown in Table 9
TABLE 9 results of tests for impurity content, particle size distribution and flowability before and after modification of metal powder
The embodiments of the present invention have been described in detail above, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, and yet fall within the scope of the invention.
Claims (7)
1. The nano modification method for the surface of the metal powder is characterized by comprising the following steps of:
adding a metal powder raw material into a ball mill, vacuumizing the ball mill to a vacuum degree of not higher than 0.01Pa, introducing inert gas into the ball mill, heating to 100-500 ℃, preserving heat for 1-5 hours, modifying the surface of the metal powder by growing a nano layer in situ on the surface of the metal powder in the high-temperature heat treatment process, naturally cooling, and screening the cooled material to obtain a finished product;
the metal powder raw material is alloy powder subjected to gas atomization treatment or simple substance metal powder subjected to gas atomization treatment;
the particle size of the metal powder raw material is not more than 150 μm.
2. The method of claim 1, wherein the alloy powder is selected from one or more of nickel-based alloy powder, aluminum-based alloy powder, cobalt-based alloy powder, stainless steel powder, and die steel alloy powder.
3. The method for nano-modifying a surface of a metal powder according to claim 1, wherein the inert gas is one or more selected from the group consisting of nitrogen, argon and helium.
4. The method for nano-modifying a metal powder surface according to claim 1, wherein the ball mill has a gas pressure of 1.0 x 10 after introducing an inert gas 5 ～1.5×10 5 Pa。
5. The method for nano-modification of metal powder surface according to claim 1, wherein the step of screening the cooled material comprises: firstly removing the material with the granularity smaller than 15 mu m, and then selecting the material with the granularity smaller than 53 mu m.
6. The method of claim 1, wherein the final product is spherical or nearly spherical in shape.
7. A metal powder for 3D printing, which is produced by the metal powder surface nano-modification method according to any one of claims 1 to 6.
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