WO2022041258A1 - 一种用于3d打印的纳米陶瓷金属复合粉末及应用 - Google Patents
一种用于3d打印的纳米陶瓷金属复合粉末及应用 Download PDFInfo
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- WO2022041258A1 WO2022041258A1 PCT/CN2020/112701 CN2020112701W WO2022041258A1 WO 2022041258 A1 WO2022041258 A1 WO 2022041258A1 CN 2020112701 W CN2020112701 W CN 2020112701W WO 2022041258 A1 WO2022041258 A1 WO 2022041258A1
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- 239000000843 powder Substances 0.000 title claims abstract description 233
- 239000000919 ceramic Substances 0.000 title claims abstract description 149
- 239000002905 metal composite material Substances 0.000 title claims description 51
- 238000007639 printing Methods 0.000 title description 2
- 239000002245 particle Substances 0.000 claims abstract description 132
- 239000002131 composite material Substances 0.000 claims abstract description 97
- 238000010146 3D printing Methods 0.000 claims abstract description 75
- 238000000498 ball milling Methods 0.000 claims abstract description 59
- 238000000034 method Methods 0.000 claims abstract description 51
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 42
- 230000008569 process Effects 0.000 claims abstract description 35
- 239000002994 raw material Substances 0.000 claims abstract description 33
- 238000005516 engineering process Methods 0.000 claims abstract description 31
- 239000000463 material Substances 0.000 claims abstract description 27
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 20
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 19
- 239000000956 alloy Substances 0.000 claims abstract description 19
- 239000000758 substrate Substances 0.000 claims abstract description 11
- 239000011261 inert gas Substances 0.000 claims description 31
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- 238000009827 uniform distribution Methods 0.000 claims description 27
- 238000001238 wet grinding Methods 0.000 claims description 25
- 238000009837 dry grinding Methods 0.000 claims description 22
- 229910052751 metal Inorganic materials 0.000 claims description 20
- 239000002184 metal Substances 0.000 claims description 20
- 239000000203 mixture Substances 0.000 claims description 16
- 229910000601 superalloy Inorganic materials 0.000 claims description 16
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 238000002844 melting Methods 0.000 claims description 12
- 230000008018 melting Effects 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 12
- 238000007873 sieving Methods 0.000 claims description 12
- 239000011156 metal matrix composite Substances 0.000 claims description 11
- 238000010894 electron beam technology Methods 0.000 claims description 10
- 238000002360 preparation method Methods 0.000 claims description 9
- 239000007789 gas Substances 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 6
- 239000012159 carrier gas Substances 0.000 claims description 6
- 239000000112 cooling gas Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 239000001301 oxygen Substances 0.000 claims description 6
- 229910052760 oxygen Inorganic materials 0.000 claims description 6
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
- 239000007769 metal material Substances 0.000 claims description 4
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 4
- 150000002910 rare earth metals Chemical class 0.000 claims description 4
- 229910000881 Cu alloy Inorganic materials 0.000 claims description 2
- 229910000640 Fe alloy Inorganic materials 0.000 claims description 2
- 229910000861 Mg alloy Inorganic materials 0.000 claims description 2
- 229910000990 Ni alloy Inorganic materials 0.000 claims description 2
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 229910000838 Al alloy Inorganic materials 0.000 claims 1
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 abstract description 3
- 229910033181 TiB2 Inorganic materials 0.000 abstract description 3
- 230000002787 reinforcement Effects 0.000 abstract description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000011159 matrix material Substances 0.000 description 25
- 238000009826 distribution Methods 0.000 description 14
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 12
- 229910010271 silicon carbide Inorganic materials 0.000 description 12
- 238000004519 manufacturing process Methods 0.000 description 10
- 239000000155 melt Substances 0.000 description 10
- 230000003014 reinforcing effect Effects 0.000 description 10
- 238000012360 testing method Methods 0.000 description 10
- 239000000654 additive Substances 0.000 description 9
- 230000000996 additive effect Effects 0.000 description 9
- 229910003407 AlSi10Mg Inorganic materials 0.000 description 8
- 238000005054 agglomeration Methods 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 6
- 229910052782 aluminium Inorganic materials 0.000 description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 5
- 230000008676 import Effects 0.000 description 5
- 239000011148 porous material Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000002105 nanoparticle Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000007712 rapid solidification Methods 0.000 description 3
- 230000008707 rearrangement Effects 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 229910000542 Sc alloy Inorganic materials 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 2
- 239000011230 binding agent Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000005728 strengthening Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
Classifications
-
- B22F1/0003—
-
- 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
- B22F1/14—Treatment of metallic powder
-
- 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
-
- 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
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/25—Process efficiency
Definitions
- the invention provides a nano-ceramic metal composite powder for 3D printing and application thereof, belonging to the technical field of metal matrix composite materials and additive manufacturing.
- Ceramic-reinforced metal matrix composites have the advantages of high specific strength, specific modulus, high temperature resistance, small thermal expansion coefficient, wear resistance, corrosion resistance, and good dimensional stability. Nano-ceramic reinforced metal matrix composites can maintain good toughness while improving mechanical properties such as strength and hardness.
- additive Manufacturing (AM) technology is a technology that accumulates and superimposes materials point by point and layer by layer to form a three-dimensional entity through the principle of discrete-accumulation.
- SLM selective laser melting
- EBM electron beam melting
- LENS coaxial powder feeding laser forming
- 3D printing technology to prepare nano-ceramic reinforced metal matrix composite materials can simplify and shorten the processing process, form three-dimensional complex structural parts at one time, and save raw material loss.
- the 3D printing of nano-ceramic reinforced metal matrix composites has the following difficulties: (1) 3D printing technology has high requirements on the sphericity, fluidity and particle size distribution of raw material powders.
- Chinese patent (CN111168057A) discloses a nano-ceramic reinforced high-entropy alloy composite powder for additive manufacturing and its preparation method and application.
- the high-entropy alloy is used as the matrix powder, and the nano-ceramic particles are used as the reinforcing phase particles.
- Ultrasonic dispersion + mechanical The high-entropy alloy powder with the nano-ceramic particles uniformly adhered on the surface is obtained by stirring, and then the spherical nano-ceramic particle-reinforced high-entropy alloy composite powder is prepared by the radio frequency plasma spheroidization technology.
- Chinese patent (CN108480625A) discloses a silicon carbide particle reinforced aluminum matrix composite forming method based on selective laser melting technology. The method includes: (1) selecting spherical AlSi10Mg powder with a purity of more than 99.9% and an average particle size distribution of 30 ⁇ m; 99.9% or more SiC powder with an average particle size distribution of 10 ⁇ m; (2) the above two powders are uniformly mixed by a powder mixer without destroying the sphericity of the aluminum matrix powder, wherein the weight of the SiC powder accounts for the total weight of the mixed powder 8 ⁇ 12%.
- the uniformly mixed powder is used for selective laser melting and forming, and a high-density silicon carbide particle reinforced aluminum matrix composite material is successfully prepared by controlling the thickness of the powder layer and process regulation.
- the powder will not be deformed and broken during the powder mixing process in the mixer, so the silicon carbide particle reinforcing phase in the prepared composite material still maintains an average particle size of about 10 ⁇ m.
- the invention proposes for the first time that nanometer ceramic metal spherical composite powder is prepared by using micron-scale ceramic particles as raw materials, and a nanometer ceramic reinforced metal composite material is prepared by 3D printing technology.
- micron-sized ceramic particles as raw materials, through a specific ball milling process, plasma spheroidization, airflow classification and sieving, a metal composite powder with high sphericity, good fluidity and narrow particle size range is obtained. Higher requirements for powders; nano-ceramic reinforced metal composites are prepared by 3D printing technology.
- the Marangoni convection is used to stir the melt, which promotes the rearrangement of ceramic particles in the melt, realizes the uniform distribution of nano-ceramic phases in the melt, solves the problem of nano-ceramic phase agglomeration, and rapidly solidifies to obtain nano-ceramics Solidification structure with uniform phase distribution; high temperature melting and rapid solidification by laser or electron beam to solve the problem of interface defects caused by poor wettability between the ceramic reinforcing phase and the metal matrix; using micron-sized ceramic particles to achieve uniform dispersion through nanometerization , low cost; can be integrally formed to prepare parts of any complex shape, and improve the utilization rate of materials.
- the prepared metal composite material has uniform nano-ceramic phase distribution and excellent mechanical properties.
- the present invention proposes a nano-ceramic metal composite powder for 3D printing and its application. Using micron-scale ceramic particles as raw materials, nano-ceramic metal spherical composite powder is prepared, and nano-ceramic reinforced composite powder is prepared by 3D printing technology. Metal composites.
- micron-sized ceramic particles as raw materials, through a specific ball milling process, plasma spheroidization, airflow classification and sieving, a metal composite powder with high sphericity, good fluidity and narrow particle size range is obtained. Higher requirements for powders; nano-ceramic reinforced metal composites are prepared by 3D printing technology.
- the Marangoni convection is used to stir the melt, which promotes the rearrangement of ceramic particles in the melt, realizes the uniform distribution of nano-ceramic phases in the melt, solves the problem of nano-ceramic phase agglomeration, and rapidly solidifies to obtain nano-ceramics Solidification structure with uniform phase distribution; high temperature melting and rapid solidification by laser or electron beam to solve the problem of interface defects caused by poor wettability between the ceramic reinforcing phase and the metal matrix; using micron-sized ceramic particles to achieve uniform dispersion through nanometerization , low cost; can be integrally formed to prepare parts of any complex shape, and improve the utilization rate of materials.
- the prepared metal composite material has uniform nano-ceramic phase distribution and excellent mechanical properties.
- a nano-ceramic metal composite powder for 3D printing of the present invention is prepared by the following scheme, and the scheme includes the following steps.
- Preparation of composite powder take micron ceramic particles as raw material A and metal powder as raw material B; first wet and then dry-grind raw material A and part of raw material B to obtain composite powder C with uniform distribution of nano-ceramic particles .
- the present invention is a preparation method of nano-ceramic metal composite powder for 3D printing.
- the mass ratio of the raw material A and the raw material B is: (0.5-10): (100-90);
- the metal powder B is selected from aluminum One of alloys, copper alloys, magnesium alloys, rare earth-containing nickel alloys, nickel-based superalloys, iron alloys, and high-entropy alloys;
- the particle size of the metal material powder is 15-53 ⁇ m or 53-106 ⁇ m.
- the micro-scale ceramic particles are selected from at least one of TiC, SiC, TiB 2 , WC, A1 2 O 3 , Y 2 O 3 , and TiO 2 ; the micro-scale ceramic particles have a particle size of 1-10 ⁇ m.
- the present invention is a preparation method of nano-ceramic metal composite powder for 3D printing.
- step (1) raw material A and part of raw material B are first wet-milled and then dry-milled.
- raw material A and used The mass ratio of raw material B is 1:1 to 1:5.
- the present invention provides a method for preparing nano-ceramic metal composite powder for 3D printing.
- step (1) firstly, micron-scale ceramic particles are crushed by wet grinding to obtain composite powder with uniform distribution of nano-ceramic particles; Water ethanol is used as the ball milling medium.
- the ball milling parameters are: the ratio of ball to material is 10:1 to 5:1, the ball milling speed is 150 to 300 rpm, and the ball milling time is 5 to 20 hours.
- the dry grinding process is carried out in an inert gas, and the ball milling parameters are: the ratio of ball to material is 5:1 to 1:1, the ball milling speed is 100 ⁇ 200rpm, and the ball milling time is 2 ⁇ 10h.
- the present invention provides a method for preparing nano-ceramic metal composite powder for 3D printing, wherein the plasma spheroidization parameters are: the flow rate of the carrier gas is 0.2-1.5 m 3 /h, the flow rate of the plasma argon gas is 0.5-3 m 3 /h, The cooling gas flow rate is 1-6 m 3 /h, and the powder feeding rate is 1-5 kg/h.
- the present invention is a nano-ceramic metal composite powder for 3D printing and its application.
- the mixed powder F is formed by 3D printing technology to prepare a nano-ceramic particle reinforced metal matrix composite material; the 3D printing is selective laser melting (SLM). , Electron beam melting (EBM), coaxial powder feeding laser forming (LENS) technology.
- SLM selective laser melting
- EBM Electron beam melting
- LENS coaxial powder feeding laser forming
- the invention relates to a nano-ceramic metal composite powder for 3D printing and its application.
- the 3D printing process is as follows: establishing a three-dimensional CAD model on a computer according to the shape of the part; using software to slice and layer the model and import it into an additive manufacturing system; Through the numerical control system, the mixed powder F is scanned reciprocally by the focused high-energy laser or electron beam according to the determined scanning route, and the powder is spread layer by layer, fused, and superimposed layer by layer until a three-dimensional part is formed.
- the invention relates to a nano-ceramic metal composite powder for 3D printing and its application.
- the mixed powder F needs to be dried at 60-150° C. for 2-12 hours in a vacuum or an inert atmosphere.
- the invention relates to a nano-ceramic metal composite powder for 3D printing and its application.
- the substrate used in the 3D printing is a stainless steel substrate or a similar metal material substrate.
- the present invention is a nano-ceramic metal composite powder for 3D printing and its application.
- the 3D printing technology adopts SLM, and the process parameters are as follows: the diameter of the laser spot is 70-110 ⁇ m, the laser power is 150-400W, and the laser scanning rate is 500-1300mm/s , the laser scanning spacing is 60-120 ⁇ m, and the thickness of the powder layer is 30-50 ⁇ m.
- the inert gas should be helium, argon, or a mixed gas of argon and helium, with a purity of 99.99 wt %, wherein the oxygen content is less than 0.0001 wt %.
- the present invention proposes a nano-ceramic-metal composite powder for 3D printing and its application.
- Micro-ceramic particles are used as raw materials, mixed with matrix alloy powder, and ball-milled by a specific ball milling process, so that the micro-ceramic particles are broken and nano-sized. , and is evenly coated by the base alloy powder, which effectively solves the problem of the agglomeration of nano-ceramic particles; in the process of crushing and nano-sized micro-ceramic particles, it is uniformly distributed in the base alloy powder, and a composite powder with uniform distribution of nano-ceramic particles is prepared; The conditions are provided for the uniform distribution of nano-ceramic particles in the melt.
- the present invention proposes a nano-ceramic metal composite powder for 3D printing and its application.
- the micro-ceramic particles A and part of the metal powder B are processed by wet grinding and then dry grinding to obtain a composite powder with uniform distribution of nano-ceramic particles. ;Through wet grinding, the micro-ceramic particles are quickly and uniformly broken and nano-sized; through dry grinding, the powder is further broken and uniformly dispersed; Ceramic particles A are mixed with some metal powders B and ball-milled to reduce the amount of ball-milled powder. ,Improve efficiency.
- the present invention proposes a nano-ceramic metal composite powder for 3D printing and its application.
- the metal composite powder with a uniform distribution of nano-ceramic phases is subjected to plasma spheroidization, airflow classification and screening to obtain high sphericity and good fluidity.
- Metal composite powder with a narrow particle size range of nano-ceramic uniform distribution which meets the requirements of 3D printing technology for powder and ensures the smooth progress of 3D printing.
- the present invention proposes a nano-ceramic metal composite powder for 3D printing and its application.
- the powder is wet-milled and dry-milled to obtain a metal-based composite powder with a uniform distribution of nano-ceramic phases; 3D
- the Marangoni convection is used to stir the melt, which promotes the rearrangement of ceramic particles in the melt, inhibits particle agglomeration, makes the nano-ceramic particles evenly distributed in the melt, and rapidly solidifies to obtain a solidified structure with uniform distribution of nano-ceramic phases. , improved tissue uniformity.
- the present invention proposes a nano-ceramic metal composite powder for 3D printing and its application.
- a metal matrix composite powder with uniform distribution of nano-ceramic phases is obtained.
- powder which greatly improves the bonding force between the nano-ceramic phase and the metal matrix; through the high temperature melting and rapid solidification of laser or electron beam, the problem of interface defects caused by poor wettability between the reinforcing phase and the metal matrix is solved, and the prepared composite material is
- the enhanced phase maintains nano-characteristics, and finally produces parts with no defects, high density, fine and dense microstructure, and excellent mechanical properties.
- the present invention proposes a nano-ceramic metal composite powder for 3D printing and its application.
- the nano-ceramic phase acts as a nucleation particle, refines the grains, obtains an equiaxed grain structure, and effectively inhibits the 3D printing process.
- the present invention proposes a nano-ceramic-metal composite powder for 3D printing and its application.
- the use of 3D printing technology can solve the problem of preparing difficult-to-process materials and integral forming of complex parts, without forming molds, and shortening the manufacturing cycle and cost. .
- the present invention proposes a nano-ceramic-metal composite powder for 3D printing and its application.
- the prepared composite material has a reinforcing phase size of nanometer level, uniform distribution, good combination with the matrix, and can improve the performance of the composite material at the same time.
- the strength and plasticity of the formed part; the micro-ceramic particles adopted in the present invention have low cost, simple method and can be applied on a large scale.
- Figure 1 is a scanning electron microscope (SEM) photo of the composite powder with uniform distribution of nano-ceramic particles obtained by wet grinding and dry grinding of micron-sized ceramic particles and René 104 nickel-based superalloy powder before forming in Example 1.
- SEM scanning electron microscope
- Figure 2 is an example of a pair of composite powders prepared in step (1) with uniformly distributed nano-ceramic particles subjected to plasma spheroidization, airflow classification and sieving to obtain SEM images of metal composite powders with uniformly distributed nano-ceramics.
- Figure 3 is the particle size distribution curve of the TiC/René104 composite powder prepared in Example 1.
- Example 4 is a SEM photograph of the microstructure of the XY and XZ surfaces of the nano-ceramic phase-reinforced René 104 nickel-based superalloy bulk prepared by using the SLM technology in Example 1.
- Figure 5 is the particle size distribution curve of the TiB2/TC4 composite powder prepared in Example 3.
- Figure 6 is a SEM photograph of the morphology of the composite powder prepared in Comparative Example 4 by wet grinding and dry grinding with the parameters of step (1).
- a nano-ceramic-metal composite powder for 3D printing and its application using René104 nickel-based superalloy as a matrix, using TiC ceramic particles with an average particle size of 2.5 ⁇ m as a reinforcing phase, and adding a mass percentage of 2.0%.
- the matrix material is René104 nickel-based superalloy spherical powder with a particle size of 15-53 ⁇ m.
- the composition of René104 nickel-based superalloy is: 20.6Co ⁇ 13Cr ⁇ 3.4Al ⁇ 3.9Ti ⁇ 3.8Mo ⁇ 2.1W ⁇ 2.4Ta ⁇ 0.9Nb ⁇ 0.05Zr ⁇ 0.03B ⁇ 0.04C ⁇
- the balance is Ni.
- the nano-ceramic metal composite powder for 3D printing and its application, the steps are as follows.
- step (1) In an inert gas atmosphere, the composite powder obtained in step (1) is placed in a plasma spheroidization device for spheroidization and cooling to obtain spherical composite powder with uniform distribution of nano-ceramic particles.
- step (3) The spherical composite powder obtained in step (2) is classified by air flow and ultrasonic vibration sieving under the protection of inert gas to obtain spherical composite powder with a particle size of 15-53 ⁇ m.
- anhydrous ethanol is used as the ball milling medium, and the ball milling parameters are: the ball-to-material ratio is 7.5:1, the ball milling speed is 250 rpm, and the ball milling time is 20 h; the dry milling process is carried out in an inert gas, and the ball milling The parameters are: the ball-to-material ratio is 5:1, the ball milling speed is 150rpm, and the ball milling time is 8h.
- the plasma spheroidization parameters in the step (2) are: the flow rate of the carrier gas is 0.8m 3 /h, the flow rate of the plasma argon gas is 2.0m 3 /h, the flow rate of the cooling gas is 3.5m 3 /h, and the powder feeding rate is 4.0 kg/h.
- the SLM process parameters of the step (5) are as follows: the laser spot diameter is 70 ⁇ m, the laser power is 250 W, the laser scanning rate is 900 mm/s, the laser scanning distance is 90 ⁇ m, the thickness of the powder layer is 40 ⁇ m, and the substrate heating temperature is 200 ° C.
- the inert gas is argon, the purity is 99.99wt%, and the oxygen content is less than 0.0001wt%.
- Figure 1 is a scanning electron microscope (SEM) photograph of the morphology of the composite powder with uniform distribution of nano-ceramic particles obtained by wet grinding and dry grinding of micron-scale ceramic particles and René 104 alloy powder before forming in Example 1. It can be observed that the micro-scale TiC ceramic particles are broken into nano-sized, and together with the matrix René 104 alloy powder, a composite powder with uniform distribution of nano-ceramic particles is formed.
- SEM scanning electron microscope
- Figure 2 is an example of a pair of composite powders prepared in step (1) with uniformly distributed nano-ceramic particles subjected to plasma spheroidization, airflow classification and sieving to obtain SEM images of metal composite powders with uniformly distributed nano-ceramics. It can be observed that after plasma spheroidization, airflow classification and sieving, the composite powder has high sphericity and uniform size.
- Figure 3 is the particle size distribution curve of the TiC/René104 composite powder prepared in Example 1. It can be seen that the average particle size of the prepared TiC/René 104 composite powder is 30.3 ⁇ m, the Dv(10) is 21.8 ⁇ m, and the Dv(90) is 52.4 ⁇ m.
- Example 4 is a SEM photograph of the microstructure of the XY and XZ surfaces of the nano-ceramic phase-reinforced René 104 nickel-based superalloy bulk prepared by using the laser 3D printing technology in Example 1. It can be observed from Figure 4 that the nano-TiC ceramic particles prepared by 3D printing are uniformly distributed in the René104 nickel-based superalloy matrix, and the prepared composite bulk has fine and uniform grains and a dense structure.
- the fluidity of the prepared TiC/René104 composite powder 50g/2.5mm aperture is 24.8s; the particle size is in the range of 15-53 ⁇ m, which can meet the SLM forming requirements.
- the yield strength of the SLM-prepared samples was 1513 MPa, the tensile strength was 1854 MPa, and the elongation was 8.6%.
- a spherical composite material is prepared by using the raw materials in a silicon carbide particle reinforced aluminum matrix composite material forming method based on the selective laser melting technology described in the Chinese patent (CN108480625A). powder, and using the SLM process parameters of the Chinese patent (CN108480625A) example, the SiC/AlSi10Mg composite material was prepared. include.
- the spherical AlSi10Mg powder with an average particle size of 30 ⁇ m is used as the matrix, and the SiC powder with an average particle size of 10 ⁇ m is used as the reinforcing particle, wherein the mass fraction of the SiC powder is 10%, and the purity of both is above 99.9%.
- the specific preparation steps are as follows.
- step (1) In an inert gas atmosphere, the composite powder obtained in step (1) is placed in a plasma spheroidization device for spheroidization and cooling to obtain spherical composite powder with uniform distribution of nano-ceramic particles.
- step (3) The spherical composite powder obtained in step (2) is classified by air flow and ultrasonic vibration sieving under the protection of inert gas to obtain spherical composite powder with a particle size of 15-53 ⁇ m.
- step (3) Mix the spherical composite powder screened in step (3) and the remaining AlSi10Mg powder under the protection of an inert gas using a V-type mixer to obtain a powder in which the spherical composite powder and the AlSi10Mg powder are uniformly mixed.
- anhydrous ethanol is used as the ball milling medium, and the ball milling parameters are: the ball-to-material ratio is 10:1, the ball milling speed is 200 rpm, and the ball milling time is 15 hours; the dry milling process is carried out in an inert gas, and the ball milling The parameters are: the ball-to-material ratio is 3:1, the ball milling speed is 200rpm, and the ball milling time is 8h.
- the plasma spheroidization parameters in the step (2) are: the flow rate of the carrier gas is 1.0m 3 /h, the flow rate of the plasma argon gas is 2.0m 3 /h, the flow rate of the cooling gas is 4.0m 3 /h, and the powder feeding rate is 3.5 kg/h.
- the SLM process parameters of the step (5) are as follows: the laser spot diameter is 100 ⁇ m, the laser power is 290 W, the laser scanning rate is 1100 mm/s, the laser scanning distance is 0.12 mm, the thickness of the powder layer is 30 ⁇ m, and the substrate heating temperature is 200 ° C.
- the inert gas is argon, the purity is 99.99wt%, and the oxygen content is less than 0.0001wt%.
- the fluidity of the prepared SiC/AlSi10Mg composite powder 50g/2.5mm pore size is 30.4s; the median particle size is 29.6 ⁇ m, which can meet the SLM forming requirements in the range of 15-53 ⁇ m.
- the density of the samples measured by Archimedes drainage method was 98.85%; the average microhardness of the prepared samples was 262 HV 0.1 , the yield strength was 354MPa, the tensile strength was 403MPa, and the elongation was 9.6%.
- the density and mechanical properties are significantly improved.
- a nano-ceramic-metal composite powder for 3D printing and its application using TC4 titanium alloy as a matrix, using TiB2 ceramic particles with an average particle size of 5 ⁇ m as a reinforcing phase, and adding a mass percentage of 2.0%.
- the matrix material is a spherical powder of TC4 titanium alloy with a particle size of 53-106 ⁇ m.
- the nano-ceramic metal composite powder for 3D printing and its application, the steps are as follows.
- step (1) In an inert gas atmosphere, the composite powder obtained in step (1) is placed in a plasma spheroidization device for spheroidization and cooling to obtain spherical composite powder with uniform distribution of nano-ceramic particles.
- step (3) The spherical composite powder obtained in step (2) is classified by air flow and ultrasonic vibration sieving under the protection of inert gas to obtain spherical composite powder with a particle size of 53-106 ⁇ m.
- step (3) Mix the spherical composite powder screened in step (3) and the remaining TC4 alloy powder with a V-type mixer under the protection of inert gas to obtain a powder in which the spherical composite powder and the TC4 alloy powder are uniformly mixed.
- anhydrous ethanol is used as the ball milling medium, and the ball milling parameters are: the ball-to-material ratio is 10:1, the ball milling speed is 200 rpm, and the ball milling time is 16 hours; the dry milling process is carried out in an inert gas, and the ball milling The parameters are: the ball-to-material ratio is 5:1, the ball milling speed is 200rpm, and the ball milling time is 8h.
- the plasma spheroidization parameters in the step (2) are: the flow rate of the carrier gas is 0.7m 3 /h, the flow rate of the plasma argon gas is 1.5m 3 /h, the flow rate of the cooling gas is 3.0m 3 /h, and the powder feeding rate is 3.0 kg/h.
- the EBM process parameters of the step (5) are as follows: the accelerating voltage is 60 kV, the electron beam current is 13.5 mA, the scanning speed is 7.6 m/s, the thickness of the powder layer is 50 ⁇ m, and the substrate heating temperature is 780 °C.
- the inert gas is argon, the purity is 99.99wt%, and the oxygen content is less than 0.0001wt%.
- Figure 5 is the particle size distribution curve of the TiB 2 /TC4 composite powder prepared in Example 3. It can be seen that the average particle size of the prepared TiB 2 /TC4 composite powder is 75.3 ⁇ m, Dv(10) is 31.4 ⁇ m, and Dv(90) is 100.6 ⁇ m.
- the fluidity of the prepared TiB 2 /TC4 composite powder 50g/2.5mm pore size is 13.5s; the median particle size is 75.3 ⁇ m, which can meet the EBM forming requirements in the range of 53-106 ⁇ m.
- the yield strength of the EBM-prepared samples was 1032 MPa, the tensile strength was 1145 MPa, and the elongation was 10.6%.
- the matrix material is a spherical powder of René104 nickel-based superalloy with a particle size of 15-53 ⁇ m and a trace amount of rare earth Sc added.
- the balance of 2.4Ta ⁇ 0.9Nb ⁇ 0.05Zr ⁇ 0.03B ⁇ 0.04C ⁇ 0.08Sc is Ni.
- the nano-ceramic metal composite powder for 3D printing and its application, the steps are as follows.
- step (1) In an inert gas atmosphere, the composite powder obtained in step (1) is placed in a plasma spheroidization device for spheroidization and cooling to obtain spherical composite powder with uniform distribution of nano-ceramic particles.
- step (3) The spherical composite powder obtained in step (2) is classified by air flow and ultrasonic vibration sieving under the protection of inert gas to obtain spherical composite powder with a particle size of 15-53 ⁇ m.
- step (3) Mix the spherical composite powder screened in step (3) with the remaining René104-Sc alloy powder under the protection of an inert gas using a V-type mixer to obtain a powder in which the spherical composite powder and the René104 nickel-based superalloy powder are uniformly mixed .
- anhydrous ethanol is used as the ball milling medium, and the ball milling parameters are: the ball-to-material ratio is 7.5:1, the ball milling speed is 250 rpm, and the ball milling time is 20 h; the dry milling process is carried out in an inert gas, and the ball milling The parameters are: the ball-to-material ratio is 5:1, the ball milling speed is 150rpm, and the ball milling time is 8h.
- the plasma spheroidization parameters in the step (2) are: the flow rate of the carrier gas is 0.8m 3 /h, the flow rate of the plasma argon gas is 2.0m 3 /h, the flow rate of the cooling gas is 3.5m 3 /h, and the powder feeding rate is 4.0 kg/h.
- the SLM process parameters of the step (5) are as follows: the laser spot diameter is 70 ⁇ m, the laser power is 225 W, the laser scanning rate is 900 mm/s, the laser scanning spacing is 90 ⁇ m, the thickness of the powder layer is 40 ⁇ m, and the substrate heating temperature is 150 ° C.
- the inert gas is argon, the purity is 99.99wt%, and the oxygen content is less than 0.0001wt%.
- the prepared TiC/René104-Sc composite powder with 50g/2.5mm pore size has a fluidity of 14.5s and a median particle size of 30.6 ⁇ m, which can meet the SLM forming requirements within the range of 15-53 ⁇ m.
- the yield strength of the SLM-prepared samples was 1521 MPa, the tensile strength was 1863 MPa, and the elongation was 11.4%.
- Example 1 The difference from Example 1 is that the step (1) only performs wet grinding treatment, and the others remain unchanged.
- the prepared TiC/René104 composite powder with 50g/2.5mm pore size has a fluidity of 38.4s and a median particle size of 36.5 ⁇ m, which can meet the SLM forming requirements within the range of 15-53 ⁇ m.
- the yield strength of the SLM preparation was 1345 MPa, the tensile strength was 1654 MPa, and the elongation was 4.6%.
- Example 1 The difference from Example 1 is that the step (1) only performs dry grinding, and the others remain unchanged.
- the prepared TiC/René104 composite powder has no fluidity after 50g/2.5mm aperture test; it cannot meet the SLM forming requirements.
- Example 1 The difference from Example 1 is that the step (1) is dry-grinding and then wet-grinding, and the rest remain unchanged.
- the prepared TiC/René104 composite powder with 50g/2.5mm pore size has a fluidity of 43.7s and a median particle size of 26.2 ⁇ m, which can meet the SLM forming requirements within the range of 15-53 ⁇ m.
- the yield strength of the SLM-prepared samples was 1385 MPa, the tensile strength was 1516 MPa, and the elongation was 3.7%.
- Example 1 The difference from Example 1 is that the step (1) is first wet-milled and then dry-milled.
- anhydrous ethanol is used as the ball-milling medium.
- the wet-milling parameters are: the ball-to-material ratio is 4:1, and the ball-milling speed is 200rpm.
- the ball milling time is 10h; the dry milling process is carried out in an inert gas, and the ball milling parameters are: the ball-to-material ratio is 10:1, the ball-milling speed is 200rpm, and the ball-milling time is 5h. Others remain unchanged.
- Figure 6 is a SEM photograph of the morphology of the composite powder prepared by wet grinding and dry grinding with the parameters of the above step (1).
- Figure 4 The micron TiC ceramic particles did not form nano-composite powder, and the spherical powder was broken due to the ball milling treatment, which significantly reduced the fluidity of the powder, which was not conducive to the subsequent plasma spheroidization, airflow classification and screening, and could not meet the requirements of 3D printing technology. High requirements for powder sphericity, fluidity and particle size distribution; cannot be used for 3D printing technology.
- step (2) does not carry out plasma spheroidization, airflow classification and screening treatment, and the others remain unchanged.
- the fluidity of the prepared TiC/René104 composite powder 50g/2.5mm aperture is 41.2s; the median particle size is 27.5 ⁇ m, in the range of 15-53 ⁇ m.
- the prepared composite powder has low sphericity, poor fluidity, and more fine powder, which is not conducive to 3D printing.
- the yield strength of the SLM-prepared sample was 1422 MPa, the tensile strength was 1810 MPa, and the elongation was 6.3%.
Abstract
Description
Claims (10)
- 一种用于3D打印的纳米陶瓷金属复合粉末的制备方法,其特征在于,包括如下步骤:(1)复合粉末制备:以微米级陶瓷颗粒为原料A,以金属粉末为原料B;先将原料A与部分原料B通过先湿磨后干磨处理,得到纳米陶瓷颗粒均匀分布的复合粉末C;(2)复合粉末等离子球化:在惰性气体氛围中,将步骤(1)得到的复合粉末C置于等离子球化装置中进行球化,冷却,得到纳米陶瓷颗粒均匀分布的球形复合粉末D;(3)粉末筛分:将步骤(2)得到的球形复合粉末D,在惰性气体保护下使用气流分级和超声震动筛分,得到粒径为15~53μm和53~106μm的球形复合粉末E;(4)粉末均匀混合:将步骤(3)筛选的球形复合粉末E与剩余的原料B,在惰性气体保护下使用V型混料机混合,得到球形复合粉末E与金属粉末B均匀混合的粉末F。
- 根据权利要求1所述的一种用于3D打印的纳米陶瓷金属复合粉末的制备方法,其特征在于:所述原料A与原料B的质量比为:(0.5-10):(100-90);所述金属粉末B选自铝合金、铜合金、镁合金、含稀土镍合金、镍基高温合金、铁合金、高熵合金中的一种;所述金属材料粉末的粒径为15~53μm或53~106μm;所述微米级陶瓷颗粒选自TiC、SiC、TiB 2、WC、A1 2O 3、Y 2O 3、TiO 2中的至少一种;所述微米级陶瓷颗粒的粒径为1~10μm。
- 根据权利要求1所述的一种用于3D打印的纳米陶瓷金属复合粉末的制备方法,其特征在于:步骤(1)中先将原料A与部分原料B通过先湿磨后干磨处理,步骤(1)中,原料A与所用原料B的质量比为1:1~1:5。
- 根据权利要求1所述的一种用于3D打印的纳米陶瓷金属复合粉末的制备方法,其特征在于:步骤(1)中先通过湿磨处理使微米级陶瓷颗粒破碎,得到纳米陶瓷颗粒均匀分布的复合粉末;湿磨过程以无水乙醇作为球磨介质,球磨参数为:球料比为10:1~5:1,球磨转速为150~300rpm,球磨时间为5~20h;通过干磨处理使前面湿磨团聚的复合粉末分散,干磨过程在惰性气体中进行,球磨参数为:球料比5:1~1:1,球磨转速为100~200rpm,球磨时间为2~10h。
- 根据权利要求1所述的一种用于3D打印的纳米陶瓷金属复合粉末的制备方法,其特征在于,所述等离子球化参数为:运载气体流量为0.2~1.5m 3/h,等离子氩气流量为0.5~3m 3/h,冷却气体流量为1~6m 3/ h,粉末进料速率为1~5kg/h。
- 根据权利要求1-5任意一项所述的一种用于3D打印的纳米陶瓷金属复合粉末及应用,其特征在于:采用3D打印技术对混合粉末F进行成形,制备得到纳米陶瓷颗粒增强金属基复合材料;所述3D打印为选区激光熔融(SLM)技术、电子束熔化(EBM)技术、同轴送粉激光成形(LENS)技术中的一种。
- 根据权利要求6所述的一种用于3D打印的纳米陶瓷金属复合粉末及应用,其特征在于,所述3D打印过程为:根据零件形状在计算机上建立三维CAD模型;利用软件将模型切片分层,并导入增材制造系统;通过数控系统,利用聚焦的高能激光或电子束对混合粉末F按确定的扫描路线往复扫描,逐层铺粉、熔凝,层层叠加,直至形成三维零件。
- 根据权利要求6所述的一种用于3D打印的纳米陶瓷金属复合粉末及应用,其特征在于:3D打印前需对混合粉末F在真空或惰性气氛中60-150℃干燥2-12h。
- 根据权利要求6所述的一种用于3D打印的纳米陶瓷金属复合粉末及应用,其特征在于:3D打印所用的基板为不锈钢基板或同类金属材料基板。
- 根据权利要求6所述的一种用于3D打印的纳米陶瓷金属复合粉末及应用,其特征在于:所述3D打印技术采用SLM,工艺参数如下:激光光斑直径70~110μm,激光功率150~400W,激光扫描速率500~1300mm/s,激光扫描间距60~120μm,铺粉层厚为30~50μm。所述的惰性气体应为氦气、氩气,或氩、氦混合气体,纯度为99.99wt%,其中氧含量小于0.0001wt%。
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