CN114226753A - Boron nitride in-situ composite reinforced metal additive integrated manufacturing method - Google Patents
Boron nitride in-situ composite reinforced metal additive integrated manufacturing method Download PDFInfo
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- CN114226753A CN114226753A CN202111527156.1A CN202111527156A CN114226753A CN 114226753 A CN114226753 A CN 114226753A CN 202111527156 A CN202111527156 A CN 202111527156A CN 114226753 A CN114226753 A CN 114226753A
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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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
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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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/30—Process control
- B22F10/32—Process control of the atmosphere, e.g. composition or pressure in a building chamber
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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
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/30—Process control
- B22F10/36—Process control of energy beam parameters
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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
- B33Y10/00—Processes of additive manufacturing
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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
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention belongs to the technical field of additive manufacturing, and particularly relates to a metal additive integrated manufacturing method for boron nitride in-situ composite reinforcement. In the process of printing and molding metal powder, boron-containing powder and a nitrogen-containing raw material are catalyzed on the surface of molten metal powder to react in situ to generate a boron nitride nanostructure array, and the boron nitride nanostructure array is embedded in the metal piece while the metal piece is printed, so that an integrally molded boron nitride in-situ composite reinforced metal forming piece is obtained. According to the invention, the metal powder is used as a catalyst, the high temperature generated by a printing heat source enables the boron-containing powder to react with the nitrogen-containing gas in the protective gas, and the boron nitride nano structure is generated on the surface of the structural member in real time, so that the reinforced formed member has stronger mechanical property and radiation absorption capacity, the purposes of weight reduction, mechanical reinforcement and radiation absorption function enhancement of the 3D printed metal member are realized, and the method can be applied to the fields of aerospace, structural material reinforcement, radiation-proof materials and the like.
Description
Technical Field
The invention belongs to the technical field of additive manufacturing, and particularly relates to a metal additive integrated manufacturing method for boron nitride in-situ composite reinforcement.
Background
Additive manufacturing is a comprehensive technology relating to subjects such as mechanical engineering, electronic engineering, materials science, industrial design and computer science, has high manufacturing speed, high processing precision and more material saving, has greater advantages in the processing and manufacturing aspects of tiny and complex workpieces, and is widely applied to the fields of aerospace, biomedicine, engines and the like at present. As one of the foremost and most potential technologies in the whole additive manufacturing system, the metal additive manufacturing technology is an important sign for the development of the additive manufacturing technology and is also an important development direction in the future. The selective melting of the metal is an advanced manufacturing technology integrating computer aided design, numerical control technology and additive manufacturing, and can effectively realize the additive manufacturing of the metal. The method has the advantages of high material utilization rate, shortening the development period of new products, reducing the development cost of the new products, manufacturing extremely complex structures, excellent comprehensive mechanical properties of finished products and the like. Compared with the traditional casting, the formed part manufactured by metal additive manufacturing has the advantages of low cost, fast development, light weight and the like. The addition of some "reinforcing agents" to the conventional shaped parts can significantly enhance the mechanical strength of the shaped parts and add some new functions. The common reinforcing agents include novel high-strength materials such as carbon nanotubes.
Hexagonal boron nitride (hBN) is a layered material with a structure similar to graphite, and Boron Nitride Nanotubes (BNNTs) have a structure similar to corresponding one-dimensional carbon nanotubes, and have high strength, high thermal conductivity, low density, and good electrical insulation, neutron absorption, and the like. Compared with the carbon nano tube, BNNTs has similar mechanical strength and light weight characteristics, but the high temperature resistance and the oxidation resistance of the BNNTs are superior to those of the carbon nano tube; because of the polar bond between boron (B) and nitrogen (N), the interface bonding force between the BN nano material and the polymer is superior to that of the corresponding carbon nano material, and the BN nano material is more suitable for being used as a mechanical reinforcing phase of a high molecular material; electrical insulation and neutron absorption properties are also important features of BN nanomaterials as distinguished from carbon nanomaterials. Due to the special properties, the boron nitride nano material is reported to be used in light metal aluminum and the like as a structure and function enhancing additive, and the mechanical strength and neutron absorption property of alloy parts are greatly improved.
CN112430119A discloses a method for preparing a high-porosity h-BN-based ceramic material based on a photocuring molding technology, and specifically discloses a method comprising the following steps of firstly, weighing HDDA, THFA, UDPA, PUA, n-octanol and ceramic raw materials according to volume fraction, and mixing to obtain ceramic slurry; placing the ceramic slurry on a 3D printer platform, forming a slurry film after a scraper, and curing by using ultraviolet light to obtain a single-layer ceramic blank; step three, repeating the step two to obtain a required ceramic body; taking down the ceramic blank, heating and degreasing; and step five, sintering under air pressure to obtain the h-BN based ceramic material with high porosity. According to the technical scheme, ceramic blanks with different raw material compositions and different shapes can be prepared by adopting a photocuring and 3D printing forming technology. hBN is a direct addition and there is no disclosure of the use of hexagonal boron nitride as a structural and functional enhancement additive for metal alloy materials.
CN111960811A discloses a DLP forming method of diamond/cubic boron nitride-ceramic composite material, specifically discloses a DLP forming method comprising uniformly mixing diamond or cubic boron nitride powder, ceramic powder and sintering aid; adding the mixed powder into a solution containing photosensitive resin, adding metal salt, and dissolving in the solution to prepare DLP slurry; carrying out DLP printing; and carrying out binder removal, reduction and sintering on the printed sample to obtain the DLP printing sample piece of the diamond/cubic boron nitride-ceramic composite material. According to the technical scheme, the cubic boron nitride material is obtained through additive manufacturing by directly adding the cubic boron nitride powder into the ceramic powder, but the process of combining the preparation of the boron nitride nano structure with the metal additive manufacturing is not adopted.
In summary, the prior art still lacks a method for integrating the preparation of boron nitride nanostructures into the metal additive manufacturing process to achieve the purpose of improving the mechanical strength of the formed part and enhancing the neutron absorption characteristics of the member.
Disclosure of Invention
Aiming at the defects or improvement requirements of the prior art, the invention provides a boron nitride in-situ composite reinforced metal forming part and a material increase manufacturing method thereof, and aims to improve the mechanical strength of the forming part and the neutron absorption characteristic of a reinforced member by using a boron nitride nano structure prepared in situ in real time in the printing process as a reinforcing additive of a 3D printing metal part, so that the reinforced forming part has stronger mechanical property and radiation absorption capacity.
In order to achieve the above object, according to one aspect of the present invention, a method for integrally manufacturing a metal additive with enhanced boron nitride in-situ composite is provided, in which during the process of printing and molding metal powder, boron-containing powder and a nitrogen-containing raw material are catalyzed on the surface of the molten metal powder to react in situ to generate a boron nitride nanostructure array, and the boron nitride nanostructure array is embedded in the metal piece while the metal piece is printed, so as to obtain an integrally molded metal forming piece with enhanced boron nitride in-situ composite.
(1) Carrying out slicing and layering processing on a preset formed part three-dimensional model;
(2) introducing protective gas into a printing working space of the additive manufacturing equipment to reduce the oxygen content in the air in the cavity to be less than 0.1%, wherein the protective gas contains nitrogen-containing gas;
(3) and paving metal powder on a substrate of the printing working space, paving boron-containing powder on the metal powder, heating to melt the metal powder, catalyzing the boron-containing powder to react with nitrogen-containing gas in situ to generate a boron nitride nanostructure array, embedding the boron nitride nanostructure in molten metal, and forming layer by layer according to a three-dimensional model to obtain the metal forming piece.
Preferably, the heat source for melting the metal powder in step (3) is a laser, a plasma beam, or an electron beam.
Preferably, the pressure of the printing working space in the step (2) is 100-1000 kPa.
Preferably, the boron-containing powder includes at least one of elemental boron powder, boron nitride, boric acid, boron oxide, and borate.
Preferably, the metal powder includes at least one of stainless steel-based powder, titanium and titanium alloy powder, aluminum powder, nickel-based powder, and chromium-based powder.
Preferably, the mass ratio of the metal powder to the boron-containing powder is (9-1): (1-9).
Preferably, the nitrogen-containing gas is one of nitrogen and ammonia, and preferably, the protective gas further comprises argon or hydrogen.
Preferably, the powder feeding mode of the additive manufacturing equipment is powder dusting in advance or real-time powder spraying.
Preferably, the boron nitride nanostructure is one or more of a boron nitride nanotube, a boron nitride nanowire and a boron nitride nanobelt, and the boron nitride component is hexagonal boron nitride or cubic boron nitride.
The invention has the following beneficial effects:
(1) the boron nitride nanostructure prepared in situ in real time in the printing process is used as a reinforcing additive of a 3D printing metal piece, the mechanical strength of the formed piece and the neutron absorption characteristic of a reinforcing member are improved, the reinforced formed piece has stronger mechanical property and radiation absorption capacity, the purposes of weight reduction, mechanical reinforcement and radiation absorption function enhancement of the 3D printing metal piece are achieved, and the boron nitride nanostructure can be applied to the fields of aerospace, structural material reinforcement, radiation-proof materials and the like.
(2) The method comprises the steps of selecting a laser, electron beam or plasma melting process to obtain a reinforced formed part, selecting a proper metal powder catalyst, a boron-containing raw material, a nitrogen-containing raw material, a protective gas, pressure and heat source power, printing high temperature generated by a heat source under the condition that metal powder is used as the catalyst to enable the boron-containing powder and the nitrogen-containing raw material to react to generate a boron nitride nano-structure array on the surface of the structural part in real time, repeating the process to obtain the boron nitride nano-structure reinforced metal formed part, and finally obtaining the high-performance formed part.
(3) The preparation process is scientific and reasonable, has strong operability, simple process and relatively low cost, and the prepared boron nitride nano-structure in-situ composite reinforced metal forming piece has high quality.
Drawings
FIG. 1 is a schematic diagram of the preparation process of the present invention;
FIG. 2 is an SEM photograph at 1mm of the surface of the sample obtained in example 1.
FIG. 3 is an SEM photograph of the surface of the sample obtained in example 1 at 100. mu.m.
FIG. 4 is an SEM photograph of the surface of the sample obtained in example 1 at 40 μm.
FIG. 5 is an SEM photograph of the surface of a sample obtained in example 2 at 1 mm.
FIG. 6 is an SEM photograph of the surface of a sample obtained in example 2 at 300. mu.m.
FIG. 7 is an SEM photograph of the surface of a sample obtained in example 2 at 100. mu.m.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
Example 1
A boron nitride in-situ composite reinforced metal forming piece is prepared by the following method:
(1) preparation work: and cleaning dust on the working table surface, the powder spreading scraper and the translation guide rail, installing a material receiving barrel, and wiping the laser window mirror of the machine tool clean by using absorbent cotton dipped with anhydrous alcohol. Ready to process the desired metallic powder material. And lifting the working table top to the highest position, fixing the substrate on the table top, and adjusting the positions of the substrate and the scraping strips. And closing a front bin gate, opening an 'environment purification' button in HUST 3DP software, and introducing nitrogen until the oxygen content in the air in the cavity is reduced to be below 0.1%. The working chamber was continuously purged with nitrogen and a pressure of 2KPa was applied. The STL file prepared in advance is read using software.
(2) Setting parameters: and setting parameters in the manufacturing process according to the graphic file and the metal material prepared in advance. The material used in this example was 316L stainless steel powder, the parameters of which are set as shown in table 1:
TABLE 1 parameter settings used in the examples
| Layered thickness (mm) | 0.05 | Filling space (mm) | 0.14 |
| Filling speed (mm/s) | 600 | Filling power (W) | 100 |
| Contour velocity (mm/s) | 400 | Contour power (W) | 100 |
| Facula bias (mm) | 0.1 | Number of contours (times) | 1 |
| Processing Range (mm) | 0-60 | Path planning | Strip-shaped X-Y |
(3) Preprocessing: and turning on a scanning system, a laser power switch and a red light indication button in the software, and if a red light signal appears, turning on a light emitting enable button and turning on a laser switch on the equipment. Clicking a 'powder feeding 1' button, conveying 316L of powder to the substrate, and manually controlling the powder spreading roller to scrape the powder; and clicking a 'powder feeding 2' button to spray the boron-containing powder onto the 316L powder, and manually controlling a powder spreading roller to scrape the powder to be flat, so that the mass ratio of the 316L powder to the boron-containing powder is 1: 1. And clicking a 'dust removing fan' button, and clicking a '2D' button to perform manual control processing. And (5) manually processing 3-5 layers according to the method, and observing the surface processing effect of the substrate. If the effect is good, the processing can be continued.
(4) Processing: and clicking a 3D button, and automatically controlling and processing by the equipment. The introduction of a protective gas is maintained during the process to keep the oxygen content in the working chamber below the requirements.
(5) Taking out the formed piece: and after the machining is finished, the equipment automatically stops running. And opening the bin door after the temperature in the working cavity is reduced to below 50 ℃, raising the substrate to the highest point, cleaning redundant powder in the cavity and on the surface of the formed part, and finally taking out the substrate to obtain the boron nitride in-situ composite reinforced metal formed part.
Example 2
The difference between this example and example 1 is that the mass ratio of 316L to the boron-containing powder is different, and specifically, the powder feeding amount is controlled so that the contents of 316L and the boron-containing powder are 9: 1.
FIG. 2 is an SEM photograph at 1mm of the surface of the sample obtained in example 1.
FIG. 3 is an SEM photograph of the surface of the sample obtained in example 1 at 100. mu.m.
FIG. 4 is an SEM photograph of the surface of the sample obtained in example 1 at 40 μm.
FIG. 5 is an SEM photograph of the surface of a sample obtained in example 2 at 1 mm.
FIG. 6 is an SEM photograph of the surface of a sample obtained in example 2 at 300. mu.m.
FIG. 7 is an SEM photograph of the surface of a sample obtained in example 2 at 100. mu.m.
From the comparison of the SEM images of example 1 and example 2, it can be seen that the difference in the amount of boron-containing powder affects the growth of BNNTs under otherwise identical experimental conditions. Therefore, different degrees of powder spreading can be carried out in different areas of the sample, so that BNNTs grow to different degrees, and the sample is strengthened to different degrees.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. The integrated manufacturing method of the metal additive material with the boron nitride in-situ composite reinforced is characterized in that in the process of printing and forming metal powder, boron-containing powder and a nitrogen-containing raw material are catalyzed on the surface of the molten metal powder to react in situ to generate a boron nitride nanostructure array, and the boron nitride nanostructure array is embedded in the metal piece while the metal piece is printed to obtain an integrally formed metal forming piece with the boron nitride in-situ composite reinforced.
2. The additive manufacturing method according to claim 1, comprising the steps of:
(1) carrying out slicing and layering processing on a preset formed part three-dimensional model;
(2) introducing protective gas into a printing working space of the additive manufacturing equipment to reduce the oxygen content in the air in the cavity to be less than 0.1%, wherein the protective gas contains nitrogen-containing gas;
(3) and paving metal powder on a substrate of the printing working space, paving boron-containing powder on the metal powder, heating to melt the metal powder, catalyzing the boron-containing powder to react with nitrogen-containing gas in situ to generate a boron nitride nanostructure array, embedding the boron nitride nanostructure in molten metal, and forming layer by layer according to a three-dimensional model to obtain the metal forming piece.
3. The additive manufacturing method according to claim 2, wherein the heat source for melting the metal powder in step (3) is a laser, a plasma beam, or an electron beam.
4. The additive manufacturing method according to claim 3, wherein the pressure of the printing work space in the step (2) is 100-1000 kPa.
5. The additive manufacturing method of claim 2, wherein the boron-containing powder comprises at least one of elemental boron powder, boron nitride, boric acid, boron oxide, and a borate.
6. The additive manufacturing method of claim 5, wherein the metal powder comprises at least one of a stainless steel based powder, a titanium and titanium alloy powder, an aluminum powder, a nickel based powder, and a chromium based powder.
7. The additive manufacturing method according to claim 5 or 6, wherein the mass ratio of the metal powder and the boron-containing powder is (9-1): (1-9).
8. The additive manufacturing method according to claim 2, wherein the nitrogen-containing gas is one of nitrogen and ammonia, and preferably, the shielding gas further comprises argon or hydrogen.
9. The additive manufacturing method according to claim 2, wherein the powder feeding manner of the additive manufacturing apparatus is powder dusting in advance or powder dusting in real time.
10. The additive manufacturing method of claim 1, wherein the boron nitride nanostructure is one or more of a boron nitride nanotube, a boron nitride nanowire, a boron nitride nanoribbon, and a boron nitride nanosheet, and the boron nitride composition is hexagonal boron nitride or cubic boron nitride.
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| CN114799211A (en) * | 2022-05-27 | 2022-07-29 | 华中科技大学 | In-situ metal ceramic multi-material preparation method based on powder bed melting |
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