CN114951640B - Nitride particle based on laser printing and preparation method and application thereof - Google Patents
Nitride particle based on laser printing and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses nitride particles based on laser printing and a preparation method and application thereof. The preparation method comprises the following steps: preparing laser-based printing nitride particles by taking vanadium-niobium alloy powder and FeNx powder as raw materials through a laser printing process; according to the preparation method, the FeNx powder is heated and decomposed to release a large amount of active nitrogen atoms, vanadium nitride particles and niobium nitride particles can be generated with the vanadium-niobium alloy powder, the formed nitride particles are small in size and dispersed, and the formed nitride particles are applied to the enhancement of alloy strength and can be used for effectively enhancing the alloy strength.
Description
Technical Field
The invention belongs to an alloy powder preparation method, and particularly relates to a preparation method and application of nitride particles based on laser printing.
Background
The laser metal laser printing has the characteristics of high concentration of heat source, small dilution, small heat affected zone and the like, and has the unique advantages of combining excellent material performance with an accurate manufacturing process, so that the laser metal laser printing is very suitable for manufacturing functional parts with complex space structures and spatial arrangement of tissue components.
The alloy has the characteristics of high hardness, good corrosion resistance, corrosion resistance and the like, wherein the CoCrMo alloy is a cobalt-based alloy, is also commonly called as a Stellite alloy, has good mechanical properties, has excellent wear resistance and corrosion resistance, and is widely used for manufacturing wear-resistant and corrosion-resistant products as one of common cobalt-based materials, such as: joints of the human body, artificial teeth, etc. The existing preparation methods of the alloy comprise a plasma rotating electrode materialization technology, an air atomization technology and a laser printing technology. The modern industry places higher demands on alloy strength, which requires optimization of alloy structure.
In order to further improve the strength of the alloy, the method for manufacturing nitride particles is adopted to enhance the strength of the alloy, but the prior art discloses that nitrogen is introduced into the method for manufacturing the nitride particles, and the metal target vanadium material is deposited to prepare the nitride particles to improve the strength of the alloy, but the method can intensively burn the obtained nitride to be coarse, so that the improvement of the strength of the alloy is limited.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method based on laser printing of nitride particles. The nitride prepared by the method has smaller particle size and is more dispersed, and when the nitride is used for preparing other alloy materials, the strength of the alloy can be better improved.
It is another object of the present invention to provide a laser-based printing of nitride particles.
It is a further object of the present invention to provide the use of said laser-based printed nitride particles for enhancing the strength of alloys.
Another object of the present invention is to provide a method for preparing a nitride particle reinforced alloy based on laser printing.
It is another object of the present invention to provide a laser-based printed nitride particle reinforced alloy.
In order to achieve the above object, the present invention is achieved by the following technical scheme:
a method for preparing nitride particles based on laser printing, comprising the steps of:
vanadium-niobium alloy powder and FeNx powder are used as raw materials, and a laser printing process is adopted to prepare laser printing;
wherein the mass ratio of the vanadium-niobium alloy powder to the FeNx powder is 2:1-3:1; the laser power in the laser printing process is 300-1200W, and the scanning speed is 5-15 mm/s; the diameter of the light spot is 2-3 mm.
Experiments of the inventor find that FeNx powder is heated and decomposed in the laser printing process to release a large amount of active nitrogen atoms, and the active nitrogen atoms are combined with vanadium-niobium alloy powder in a molten pool to form vanadium nitride particles and niobium nitride particles; by controlling the mass ratio of the powder feeding amount of the vanadium-niobium alloy powder and the FeNx powder in the laser printing process, the dispersed nitride particles with small particle size can be prepared, and the method can be used for improving the alloy strength. When the mass ratio of the vanadium-niobium alloy powder to the FeNx powder is too large, the prepared nitride particles are coarse, the improvement of the alloy strength is limited, and when the mass ratio of the vanadium-niobium alloy powder to the FeNx powder is too small, the prepared nitride particles are small.
The quality ratio of the vanadium-niobium alloy powder to the FeNx powder is regulated and controlled, so that the prepared vanadium nitride particles and niobium nitride particles can be further improved to improve the alloy strength. Preferably, the mass ratio of the vanadium-niobium alloy powder to the FeNx powder is 2.2:1-2.8:1.
More preferably, the mass ratio of the vanadium-niobium alloy powder to the FeNx powder is 2.35:1-2.65:1.
More preferably, the mass ratio of vanadium niobium alloy powder to FeNx powder is 2.5:1.
A preparation method of a nitride particle reinforced alloy based on laser printing comprises the following steps:
the method comprises the steps of taking vanadium-niobium alloy powder, feNx powder and alloy powder to be reinforced as raw materials, and adopting a laser printing process to prepare laser printing;
wherein the mass ratio of the vanadium-niobium alloy powder to the FeNx powder is 2:1-3:1; the laser power in the laser printing process is 300-1200W, and the scanning speed is 5-15 mm/s; the diameter of the light spot is 2-3 mm.
In general, in the vanadium-niobium alloy powder, the vanadium content is 5 to 95at.%; the niobium content is 5-95 at.%.
Preferably, the alloy powder to be reinforced may be one or more of CoCrMo alloy, titanium alloy or nickel alloy.
More preferably, the alloy powder to be reinforced may be a CoCrMo alloy.
Preferably, the FeNx powder is Fe 4 N、Fe 3 N、Fe 16 N 2 One or more of them.
Preferably, the FeNx powder is a powder having a size of 20 to 100. Mu.m.
The laser power in the laser printing process of the present invention can be selected according to the prior art. Preferably, the laser power of the laser printing process is 600-900W.
The scanning speed in the laser printing process of the invention can be selected according to the prior art. Preferably, the scanning speed of the laser printing process is 8-12 mm/s.
The amount of powder fed in the laser printing process of the invention can be selected according to the prior art. Preferably, the powder feeding flow of the alloy powder to be reinforced in the laser printing process is 10-15 g/min, the powder feeding amount of FeNx powder is 0.5-3 g/min, and the powder feeding amount of vanadium-niobium alloy powder is 1.5-9 g/min.
Preferably, in the laser printing process, the diameter of a light spot is 2-3 mm, the shielding gas and the powder feeding gas are argon, and the flow rate of the argon is 10-15L/min.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a preparation method of nitride particles based on laser printing. According to the preparation method, feNx powder is heated to decompose, a large amount of active nitrogen atoms are released, vanadium nitride particles and niobium nitride particles can be generated by the FeNx powder and the vanadium niobium alloy powder, and the formed nitride particles are small in size and dispersed. The method is applied to the enhancement of alloy strength, and in the preparation method, nitride plays a role in refining the grain size of the alloy by heterogeneous nuclear particles in the solidification process of a molten pool, so that the strength of the alloy can be effectively improved.
Drawings
FIG. 1 is a schematic illustration of the preparation of a nitride particle reinforced CoCrMo alloy according to this invention.
FIG. 2 is a scanning electron microscope image of a nitride particle reinforced CoCrMo alloy of example 4.
FIG. 3 is a scanning electron microscope image of a nitride particle reinforced CoCrMo alloy of example 5.
Detailed Description
The invention is further illustrated in detail below in connection with specific examples which are provided solely for the purpose of illustration and are not intended to limit the scope of the invention. The test methods used in the following examples are conventional methods unless otherwise specified; the materials, reagents and the like used, unless otherwise specified, are those commercially available.
In the examples, a commercially available 316 stainless steel substrate, coCrMo alloy with the trade name F799, a vanadium-niobium alloy (vanadium content: 40at.%, niobium content: 60 at.%) and Fe with an average size of 45 μm were used 4 N powder.
A schematic of the preparation of the nitride particle reinforced CoCrMo alloy in the example is shown in FIG. 1.
Example 1 (vanadium niobium alloy powder and Fe 4 N powder feeding amount mass ratio is 2:1)
A preparation method of a nitride particle reinforced alloy based on laser printing comprises the following steps:
s1, performing surface cleaning treatment such as deoiling and degreasing on a 316L stainless steel substrate;
s2, coCrMo alloy powder, vanadium-niobium alloy powder and Fe 4 N powder is put into a corresponding powder feeder;
s3, preparing the nitride particle reinforced CoCrMo alloy by adopting a laser printing process;
wherein the laser power is 750W, the scanning speed is 10mm/s, the powder feeding flow of CoCrMo powder is 12g/min, fe 4 The powder feeding amount of the N powder is 2g/min, the powder feeding amount of the vanadium-niobium alloy powder is 4g/min, the vanadium-niobium alloy powder and Fe 4 The mass ratio of the powder feeding amount of the N powder is 2:1. The diameter of the light spot is 2.5mm, the shielding gas and the powder feeding gas are argon, and the flow is 12.5L/min.
Example 2 (vanadium niobium alloy powder and Fe 4 N powder feeding quantity mass ratio is 2.2:1)
A preparation method of a nitride particle reinforced alloy based on laser printing comprises the following steps:
s1, performing surface cleaning treatment such as deoiling and degreasing on a 316L stainless steel substrate;
s2, coCrMo alloy powder, vanadium-niobium alloy powder and Fe 4 N powder is put into a corresponding powder feeder;
s3, preparing the nitride particle reinforced CoCrMo alloy by adopting a laser printing process;
wherein the laser power is 750W, the scanning speed is 10mm/s, the powder feeding flow of CoCrMo powder is 12g/min, fe 4 The powder feeding amount of the N powder is 2g/min, the powder feeding amount of the vanadium-niobium alloy powder is 4.4g/min, the vanadium-niobium alloy powder and Fe 4 The mass ratio of the powder feeding amount of the N powder is 2.2:1. The diameter of the light spot is 2.5mm, the shielding gas and the powder feeding gas are argon, and the flow is 12.5L/min.
Example 3 (vanadium niobium alloy powder and Fe 4 The mass ratio of the powder feeding amount of the N powder is 2.35:1
A preparation method of a nitride particle reinforced alloy based on laser printing comprises the following steps:
s1, performing surface cleaning treatment such as deoiling and degreasing on a 316L stainless steel substrate;
s2, coCrMo alloy powder, vanadium-niobium alloy powder and Fe 4 N powder is put into a corresponding powder feeder;
s3, preparing the nitride particle reinforced CoCrMo alloy by adopting a laser printing process;
wherein the laser power is 750W, the scanning speed is 10mm/s, the powder feeding flow of CoCrMo powder is 12g/min, fe 4 The powder feeding amount of the N powder is 2g/min, the powder feeding amount of the vanadium-niobium alloy powder is 4.7g/min, the vanadium-niobium alloy powder and Fe 4 The mass ratio of the powder feeding amount of the N powder is 2.35:1. The diameter of the light spot is 2.5mm, the shielding gas and the powder feeding gas are argon, and the flow is 12.5L/min.
Example 4 (vanadium niobium alloy powder and Fe 4 N powder feeding amount mass ratio is 2.5:1)
A preparation method of a nitride particle reinforced alloy based on laser printing comprises the following steps:
s1, performing surface cleaning treatment such as deoiling and degreasing on a 316L stainless steel substrate;
s2, coCrMo alloy powder, vanadium-niobium alloy powder and Fe 4 N powder is put into a corresponding powder feeder;
s3, preparing the nitride particle reinforced CoCrMo alloy by adopting a laser printing process;
wherein the laser power is 750W, the scanning speed is 10mm/s, the powder feeding flow of CoCrMo powder is 12g/min, fe 4 The powder feeding amount of the N powder is 2g/min, the powder feeding amount of the vanadium-niobium alloy powder is 5g/min, the vanadium-niobium alloy powder and Fe 4 The mass ratio of the powder feeding amount of the N powder is 2.5:1. The diameter of the light spot is 2.5mm, the shielding gas and the powder feeding gas are argon, and the flow is 12.5L/min.
Example 5 (vanadium niobium alloy powder and Fe 4 N powder feeding quantity mass ratio is 2.65:1)
A preparation method of a nitride particle reinforced alloy based on laser printing comprises the following steps:
s1, performing surface cleaning treatment such as deoiling and degreasing on a 316L stainless steel substrate;
s2, coCrMo alloy powder, vanadium-niobium alloy powder and Fe 4 N powder is put into a corresponding powder feeder;
s3, preparing the nitride particle reinforced CoCrMo alloy by adopting a laser printing process;
wherein the laser power is 750W, the scanning speed is 10mm/s, the powder feeding flow of CoCrMo powder is 12g/min, fe 4 The powder feeding amount of the N powder is 2g/min, the powder feeding amount of the vanadium-niobium alloy powder is 5.3g/min, the vanadium-niobium alloy powder and Fe 4 The mass ratio of the powder feeding amount of the N powder is 2.65:1. The diameter of the light spot is 2.5mm, the shielding gas and the powder feeding gas are argon, and the flow is 12.5L/min.
Example 6 (vanadium niobium alloy powder and Fe 4 N powder feeding amount mass ratio is 2.8:1)
A preparation method of a nitride particle reinforced alloy based on laser printing comprises the following steps:
s1, performing surface cleaning treatment such as deoiling and degreasing on a 316L stainless steel substrate;
s2, coCrMo alloy powder, vanadium-niobium alloy powder and Fe 4 N powder is put into a corresponding powder feeder;
s3, preparing the nitride particle reinforced CoCrMo alloy by adopting a laser printing process;
wherein the laser power is 750W, the scanning speed is 10mm/s, the powder feeding flow of CoCrMo powder is 12g/min, fe 4 The powder feeding amount of the N powder is 2g/min, the powder feeding amount of the vanadium-niobium alloy powder is 5.6g/min, and the mass ratio of the vanadium-niobium alloy powder to the FeNx powder is 2.8:1. The diameter of the light spot is 2.5mm, the shielding gas and the powder feeding gas are argon, and the flow is 12.5L/min.
Example 7 (vanadium niobium alloy powder and Fe 4 N powder feeding amount mass ratio is 3:1
A preparation method of a nitride particle reinforced alloy based on laser printing comprises the following steps:
s1, performing surface cleaning treatment such as deoiling and degreasing on a 316L stainless steel substrate;
s2, coCrMo alloy powder, vanadium-niobium alloy powder and Fe 4 N powder is put into a corresponding powder feeder;
s3, preparing the nitride particle reinforced CoCrMo alloy by adopting a laser printing process;
wherein the laser power is 750W, the scanning speed is 10mm/s, the powder feeding flow of CoCrMo powder is 12g/min, fe 4 The powder feeding amount of the N powder is 2g/min, the powder feeding amount of the vanadium-niobium alloy powder is 6g/min, the vanadium-niobium alloy powder and Fe 4 The mass ratio of the powder feeding amount of the N powder is 3:1. The diameter of the light spot is 2.5mm, the shielding gas and the powder feeding gas are argon, and the flow is 12.5L/min.
In the present invention, fe in examples 1 to 7 4 N is replaced by Fe 3 N、Fe 16 N 2 The nitride particle reinforced CoCrMo alloy with equivalent performance can also be prepared.
Comparative example 1 (vanadium niobium alloy powder and Fe 4 The mass ratio of the powder feeding amount of the N powder is 1.9:1
A preparation method of a nitride particle reinforced alloy based on laser printing comprises the following steps:
s1, performing surface cleaning treatment such as deoiling and degreasing on a 316L stainless steel substrate;
s2, coCrMo alloy powder, vanadium-niobium alloy powder and Fe 4 N powder is put into a corresponding powder feeder;
s3, preparing a control CoCrMo alloy by adopting a laser printing process;
wherein the laser power is 750W, the scanning speed is 10mm/s, the powder feeding flow of CoCrMo powder is 12g/min, fe 4 The powder feeding amount of the N powder is 2g/min, the powder feeding amount of the vanadium-niobium alloy powder is 3.8g/min, the vanadium-niobium alloy powder and Fe 4 The mass ratio of the powder feeding amount of the N powder is 1.9:1. The diameter of the light spot is 2.5mm, the shielding gas and the powder feeding gas are argon, and the flow is 12.5L/min.
Comparative example 2 (vanadium niobium alloy powder and Fe 4 The mass ratio of the powder feeding amount of the N powder is 3.2:1
A preparation method of a nitride particle reinforced alloy based on laser printing comprises the following steps:
s1, performing surface cleaning treatment such as deoiling and degreasing on a 316L stainless steel substrate;
s2, coCrMo alloy powder, vanadium-niobium alloy powder and Fe 4 N powder is put into a corresponding powder feeder;
s3, preparing a control CoCrMo alloy by adopting a laser printing process;
wherein the laser power is 750W, the scanning speed is 10mm/s, the powder feeding flow of CoCrMo powder is 12g/min, fe 4 The powder feeding amount of the N powder is 2g/min, the powder feeding amount of the vanadium-niobium alloy powder is 6.4g/min, the vanadium-niobium alloy powder and Fe 4 The mass ratio of the powder feeding amount of the N powder is 3.2:1. The diameter of the light spot is 2.5mm, the shielding gas and the powder feeding gas are argon, and the flow is 12.5L/min.
Comparative example 3
A method of preparing a control alloy comprising the steps of:
s1, performing surface cleaning treatment such as deoiling and degreasing on a 316L stainless steel substrate;
s2, placing CoCrMo alloy powder into a powder feeder;
s3, processing by adopting a laser printing process to obtain a control CoCrMo alloy;
wherein, the laser power is 750W, the scanning speed is 10mm/s, and the powder feeding flow of CoCrMo powder is 12g/min. The diameter of the light spot is 2.5mm, the shielding gas and the powder feeding gas are argon, and the flow is 12.5L/min.
Experiment 1: analysis of surface topography
The nitride particle-reinforced CoCrMo alloys prepared in examples 1 to 7 above and the control CoCrMo alloys in comparative examples 1 to 3 were subjected to morphology analysis, and analyzed using a hitachi S-4300S scanning electron microscope. The results of analysis of the surface morphology of the comparative CoCrMo alloys prepared in examples 1 to 7 and comparative examples 1 to 3 are shown in table 1, and the scanning electron microscope images of the nitride particle reinforced CoCrMo alloys of example 4 and example 5 are shown in fig. 2 to 3. Wherein the volume fraction is measured according to E1245 using image analysis.
TABLE 1
The size and volume fraction of the precipitated phases in the alloy are two important factors affecting the strength of the alloy. Too large nitride particles may decrease the strength of the alloy; the higher the volume fraction of nitride particles, the higher the strength of the alloy. As can be seen from Table 1, in comparative examples 1 to 3, when the powder feed amount mass ratio of the vanadium niobium alloy powder and the FeNx powder is too low, the comparative CoCrMo alloy prepared has not more than 6nm of nitride particles, but the strength improvement of the CoCrMo alloy is poor because the size is too small and the volume fraction is less than 0.5%; when the mass ratio of the powder feeding amount of the vanadium-niobium alloy powder to the powder feeding amount of the FeNx powder is too high, the prepared contrast CoCrMo alloy has larger nitride particles, the size is larger than 50nm, the volume fraction is 5.79 percent, and the strength improvement of the CoCrMo alloy is poor due to the larger nitride particles although the volume fraction is larger; comparative example 3 does not contain nitride and cannot improve the strength of CoCrMo alloy.
As can be seen from fig. 2 and 3, the size of the nitride particles in the nitride particle reinforced CoCrMo alloy prepared in example 4 is smaller, while the size of the nitride particles in the nitride particle reinforced CoCrMo alloy prepared in example 5 is increased somewhat.
Experiment 2: tensile Strength test
The nitride particle-reinforced CoCrMo alloys prepared in examples 1 to 7 and the control CoCrMo alloys in comparative examples 1 to 3 were measured by a uniaxial tensile test using an MTS E40 universal tester, and the measurement results are shown in table 2.
TABLE 2
As can be seen from Table 2, the tensile strength of the nitride particle reinforced CoCrMo alloy prepared by the method of the present invention is not lower than 528MPa. Comparative example 3, which does not contain nitride particles, has a tensile strength of only 435.9MPa; the tensile strength of the comparative CoCrMo alloys prepared in comparative examples 1 to 2 was 454.3MPa and 509.8Pa, respectively, and although the tensile strength of the CoCrMo alloys could be improved, the improvement effect was not good because the tensile strength of the comparative CoCrMo alloys prepared was still poor because the nitride particles obtained during the preparation were too small or too large and the content of the nitride particles was affected when the powder feed amount mass ratio of the vanadium niobium alloy powder and the FeNx powder was too low or too high. As can be seen from comparing the nitride particle reinforced CoCrMo alloys prepared in examples 1-7, the tensile strength of the nitride particle reinforced CoCrMo alloy can be further improved by further adjusting the mass ratio of the powder feeding amount of the vanadium-niobium alloy powder to the powder feeding amount of the FeNx powder, and when the mass ratio of the powder feeding amount of the vanadium-niobium alloy powder to the powder feeding amount of the FeNx powder is 2.35:1-2.65:1, the tensile strength of the nitride particle reinforced CoCrMo alloy prepared is not lower than 689.9MPa; the tensile strength of the prepared nitride particle reinforced CoCrMo alloy is 713.5MPa when the mass ratio of the powder feeding amount of the vanadium-niobium alloy powder to the powder feeding amount of the FeNx powder is 2.5:1.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (10)
1. A method for preparing nitride particles based on laser printing, comprising the steps of:
vanadium-niobium alloy powder and FeNx powder are used as raw materials and are prepared by a laser printing process;
wherein the mass ratio of the vanadium-niobium alloy powder to the FeNx powder is 2:1-3:1; the laser power in the laser printing process is 300-1200W, and the scanning speed is 5-15 mm/s; the diameter of the light spot is 2-3 mm.
2. The method for preparing nitride particles based on laser printing according to claim 1, wherein the mass ratio of vanadium-niobium alloy powder to FeNx powder is 2.2:1-2.8:1.
3. The method for preparing nitride particles based on laser printing according to claim 1, wherein the mass ratio of vanadium-niobium alloy powder to FeNx powder is 2.35:1-2.65:1.
4. The method for preparing nitride particles based on laser printing according to claim 1, wherein the mass ratio of vanadium-niobium alloy powder to FeNx powder is 2.5:1.
5. The method for producing nitride particles based on laser printing according to claim 1, wherein the FeNx powder is a powder having a size of 20 to 100 μm.
6. The method for producing nitride particles based on laser printing according to claim 1, wherein the FeNx powder is Fe 4 N、Fe 3 N、Fe 16 N 2 One or more of them.
7. A laser-based printing of nitride particles, characterized in that it is produced by the production method according to any one of claims 1 to 6.
8. Use of laser-based printed nitride particles according to claim 7 for strengthening alloy strength.
9. The preparation method of the nitride particle reinforced alloy based on laser printing is characterized by comprising the following steps of:
the vanadium-niobium alloy powder, the FeNx powder and the alloy powder to be reinforced are used as raw materials and are prepared by a laser printing process;
wherein the mass ratio of the vanadium-niobium alloy powder to the FeNx powder is 2:1-3:1; the laser power in the laser printing process is 300-1200W, and the scanning speed is 5-15 mm/s; the diameter of the light spot is 2-3 mm.
10. A laser-based nitride particle reinforced alloy prepared by the method of claim 9.
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| CN110760762A (en) * | 2019-12-16 | 2020-02-07 | 江苏金物新材料有限公司 | Method for preparing mold material by 3D printing |
| CN110777276A (en) * | 2019-10-23 | 2020-02-11 | 广东工业大学 | Method for enhancing performance of alloy by using aluminum oxide based on laser 3D printing |
| WO2022067395A1 (en) * | 2020-10-02 | 2022-04-07 | Deakin University | Boron nitride nanotube modified metal powder for additive manufacturing |
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| US9399256B2 (en) * | 2014-06-20 | 2016-07-26 | Velo3D, Inc. | Apparatuses, systems and methods for three-dimensional printing |
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| AU2004321077A1 (en) * | 2004-06-10 | 2006-01-05 | Allomet Corporation | Method for consolidating tough coated hard powders |
| CN101817081A (en) * | 2010-04-30 | 2010-09-01 | 西南交通大学 | Method for preparing porous iron-based alloy material |
| CN110777276A (en) * | 2019-10-23 | 2020-02-11 | 广东工业大学 | Method for enhancing performance of alloy by using aluminum oxide based on laser 3D printing |
| CN110760762A (en) * | 2019-12-16 | 2020-02-07 | 江苏金物新材料有限公司 | Method for preparing mold material by 3D printing |
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