CA3138388A1 - Additive manufacturing powders with improved physical characteristics, method of manufacture and use thereof - Google Patents
Additive manufacturing powders with improved physical characteristics, method of manufacture and use thereof Download PDFInfo
- Publication number
- CA3138388A1 CA3138388A1 CA3138388A CA3138388A CA3138388A1 CA 3138388 A1 CA3138388 A1 CA 3138388A1 CA 3138388 A CA3138388 A CA 3138388A CA 3138388 A CA3138388 A CA 3138388A CA 3138388 A1 CA3138388 A1 CA 3138388A1
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- Prior art keywords
- particles
- additive manufacturing
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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
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/052—Metallic powder characterised by the size or surface area of the particles characterised by a mixture of particles of different sizes or by the particle size distribution
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- B22—CASTING; POWDER METALLURGY
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/06—Metallic powder characterised by the shape of the particles
- B22F1/065—Spherical particles
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/10—Metallic powder containing lubricating or binding agents; Metallic powder containing organic material
- B22F1/102—Metallic powder coated with organic material
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- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/14—Treatment of metallic powder
- B22F1/145—Chemical treatment, e.g. passivation or decarburisation
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- 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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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/30—Process control
- B22F10/38—Process control to achieve specific product aspects, e.g. surface smoothness, density, porosity or hollow structures
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/60—Treatment of workpieces or articles after build-up
- B22F10/66—Treatment of workpieces or articles after build-up by mechanical means
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- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/70—Recycling
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- B22F12/00—Apparatus or devices specially adapted for additive manufacturing; Auxiliary means for additive manufacturing; Combinations of additive manufacturing apparatus or devices with other processing apparatus or devices
- B22F12/60—Planarisation devices; Compression devices
- B22F12/67—Blades
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/12—Making metallic powder or suspensions thereof using physical processes starting from gaseous material
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
- B22F9/14—Making metallic powder or suspensions thereof using physical processes using electric discharge
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/10—Processes of additive manufacturing
- B29C64/141—Processes of additive manufacturing using only solid materials
- B29C64/153—Processes of additive manufacturing using only solid materials using layers of powder being selectively joined, e.g. by selective laser sintering or melting
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y10/00—Processes of additive manufacturing
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- B33Y70/00—Materials specially adapted for additive manufacturing
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- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3D 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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Abstract
Description
CHARACTERISTICS, METHOD OF MANUFACTURE AND USE THEREOF
CROSS-REFERENCE TO RELATED APPLICATION
[001] The present application claims the benefit of U.S. provisional patent application serial number 62/842,050 filed on May 2, 2019. The contents of the above-referenced document are incorporated herein by reference in their entirety.
TECHNICAL FIELD
BACKGROUND
Among these, van der Walls interactions, polar interactions through localized static charge and hydrogen bonding and surface tension through adsorbed water are often cited.
Of these, the static charge-mediated interactions are a non-issue in conductive powders since all charge separation is relaxed instantly as charges are free to reorganize in conductors. Van der Walls interactions are unavoidable if powders are to be handled at non-zero absolute temperatures.
Further, this known solution has a disadvantage in that it bottlenecks the production line, increases operational cost (e.g., electricity consumption) and increases likelihood of causing presence of undesirable by-products when exposing the powder to the high temperatures that are required to remove water from the powders. Further, it is extremely difficult to remove adsorb water from powder particles surface, such that some residual water often remains, which still causes powder flowability problems.
Noteworthy also is the fact that the slurring process requires large amounts of solvents which are contaminated by excess reactants (anhydrous processes use excess reactants).
Moreover, the powders need to be physically separated from the solvent and dried, which is time consuming and difficult on industrial-scale batches. Further, most of these powders do not flow in a Hall test, which is indicative that powder flowability problems remain.
Further, when inclusions are put into solution (e.g., by laser or electron-beam melting), the feedstock chemistry is altered. In view of the foregoing, this proposed solution to the flowability problem has not received market adoption.
SUMMARY
first flowability is of at least 0.90.
first flowability is of at least 0.90.
B213 at 30%
relative humidity.
BRIEF DESCRIPTION OF THE DRAWINGS
axes of two additively-manufactured parts including one additively-manufactured part manufactured with a surface-modified powder in accordance with an embodiment of the present disclosure (labeled "ST") and one additively-manufactured part manufactured with a prior-art powder with identical parameters (labeled "reg");
DETAILED DESCRIPTION
These details are provided for the purpose of non-limiting examples and the invention may be practiced according to the claims without some or all of these specific details. For the sake of clarity, technical material that is known in the technical fields related to the invention has not been described in detail so that the invention is not unnecessarily obscured.
parameters for a specific application, with current machines offering little opportunity for any form of responsive control. This means that inconsistent input material properties will translate directly into inconsistent finished parts properties. Poor powder quality can produce defects in the end part including pores, cracks, inclusions, residual stresses and suboptimal surface roughness, as well as compromising throughput. Understanding the correlations between material properties, processing performance and end component properties is therefore important, both to select the best powder for an application and to ensure the consistency of that powder, i.e., from build-to-build and layer-to-layer, as well as through recycling. Chemistry and physical characteristics of a metal powder are generally understood to define additive manufacturing performance.
Contaminant levels of just a few parts per million can be significant in terms of component quality.
B213) and/or an improved dynamic flowability as measured with a revolution powder analyzer (RPA) (e.g., "avalanche angle").
vol % a comparative powder of the prior art will typically exhibit significant disadvantages, such as reduced flowability; the chemical composition relative to BET will be too concentrated, which causes artifacts when used in 3D laser printing; when the powder is poured, fine particles create a cloud that clogs the filters inside the additive manufacturing machine and results in laser attenuation;
fine particles increase surface-to-volume ratio which will in turn increase oxygen uptake, which oxygen uptake could have adverse effects on mechanical properties such as fatigue resistance or elongation of the part. In contrast, powders of the present disclosure will show some tolerance to fine particles having a size of < 20 micrometer in levels of up to 30 vol%
fines particles in their PSD
and will not exhibit at least some of the above disadvantages.
Advantageously, powders of the present disclosure will thus have substantially the same improved physical characteristics at low and high levels of relative humidity (e.g., at any RH% in the range of from 10 RH% to 75 RH%, e.g., at 10 RtP/o and at 75 RH%, or at 30 RH% and 75 RH%).
Generally speaking, an important component of the surface roughness of parts obtained through powder based additive manufacturing is attributable to welded, un-melted powder particles attached to the part surface. In some embodiments, it is believed that this change in the wettability of the powder changes the surface tension between the melted pool and the surface of the un-melted particle, adjacent the melt pool, resulting in a higher angle of contact between the melt and the un-melted particles, which limits expansion of the metal pool and also reduces the attachment of the un-melted particles to the metal pool, as the later solidifies, thus yielding parts with improved surface finish.
The print bed containing both a printed part and un-sintered powder may weigh thousands of kilograms or more and may be difficult to handle. The person of skill will readily understand that a powder which is more fluid-like, such as the powder of the present disclosure, will more easily fall off the part when the operator retrieves the finished part from the powder bed, thus, resulting in a shortened cleaning procedure for the finished part and overall increasing productivity.
Characteristics of the powder
B213, or with an RPA
(dynamic flowability), such as the GranuDrumTM (Granutools, Belgium), which is improved relative to that one of comparative prior art powders. For example, it has been observed by the present inventors that an illustrative embodiment of the powder 10 (AlSi7Mg) has an avalanche angle of 31 degrees whereas a comparative prior art powder (AlSi7Mg) has an avalanche angle of 42 degrees.
B213 compared to that one of where the comparative prior art powder stops flowing (powder 10/comparative powder). For instance, in some embodiments, the ratio is of at least 1.05, or of at least 1.10, or of at least 1.15, or of at least 1.20, or of at least 1.25, or even more.
RH, the comparative prior art powder has an apparent density of 2.400 g/cm3 whereas this embodiment of the powder 10 has an apparent density value of about 2.480 g/cm3, again representing an increase of about 3%. At 75% RH, the comparative prior art powder has an apparent density of 2.360 g/cm3 whereas this embodiment of the powder 10 has an apparent density value of about 2.470 g/cm3, representing an increase of about 4.45%.
By doing so, finer features can be obtained as the width of the melt pool is reduced. Thus, with additional reference to Figure 35, the resolution of the 3D process may be enhanced and energy losses may be reduced. For instance, in some embodiments, for a melt pool 710 having a radius Rm of 200 !_tm and a depth Dm of 200 !_tm, a radius Rm of the molten material spread by capillary forces may be no more than 600 !_tm, in some embodiments no more than 400 !_tm, in some embodiments no more than 300 !_tm, and in some embodiments even less (e.g., no more than 250 !_tm).
Generally speaking, an important component of the surface roughness of parts obtained through powder based additive manufacturing is attributable to welded, un-melted powder particles attached to the part surface.
The herein described change in the wettability of the powder 10 by the metal allows for a high angle of contact between the melt and the cold metal particles, which prevents their inclusion at the surface and thus yields parts with improved surface finish.
indicates that this process used a powder 10 as described herein whereas the letter labeled with "2"
indicates that this process used a comparative powder of the prior art.
Without being bound by any theory, it is believed that this differential behavior can be attributed to the powder 10 being less cohesive, such that individual particles 20 are forced by the overall increased mass of material through the openings of the sieving meshes instead of forming lumps of material.
For example, for total sieved quantities ranging from 100g to 1000g, this ratio may vary by less than 0.10, or less than 0.8, or less than 0.6, or less than 0.4, or less than 0.2, or even less. For example, relatively to the recovered sieved quantity of powder 10 for a total initial quantity of 100g, in some embodiments, this ratio may vary by less than 50%, or by less than 40%, or by less than 30%, or by less than 20%, or by less than 10 /0, or by even less.
This improved separation of particles minimizes classification errors. In diminishing the cohesivity of individual powder grains, the fraction of aggregates in the gas flow is lessened. Since aggregates will behave as larger particles with lower density, they will remain with the larger fraction in the process, whereas the small particles that constitute the aggregate should not.
Powder materials
composite compounds such as forsterite, steatite, cordierite, mullite, barium titanate, lead titanate, lead zirconate titanate, Mn-Zn ferrite, Ni-Zn ferrite, and sialon; phosphate compounds such as hydroxyapatite and calcium phosphate. Of these, any species can be used singly or two or more species can be used in combination.
For example, a given powder 10 may include one or more elements such as carbon determined in accordance with ASTM
E 1941or ASTM E 1019, hydrogen determined in accordance with ASTM E 1447, oxygen and nitrogen determined in accordance with ASTM E 1409, and other elements determined in accordance with ASTM E 539 and ASTM E 2371. Other analytical methods are also known in the art and for conciseness sake, will not be further described here.
Powder particle size
0%) in accordance with ASTM B214.
Table 1 ¨ Examples of Particle size distribution for powder A
PSD Size Max.
025 > 25 gm 20%
- a m > 45 gm (325 mesh) 1 %
< 15 gm 5%
15-63 am > 63 gm (230 mesh) 10 %
> 90 gm (170 mesh) 0.2 %
<25 gm (500 mesh) 0.7 %
45-177 am <45 gm (325 mesh) 5 %
> 177 gm (80 mesh) 10 %
> 250 gm (60 mesh) 0.2 %
<25 gm (500 mesh) 0.7 %
45-106 gm <45 nm (325 mesh) 5 %
> 106 gm (140 mesh) 10 %
> 150 gm (100 mesh) 0.2 %
Table 2 - Examples of Particle size distribution for powder B
PSD Size Max.
< 20 [im 10 vol. /0 20-63 gm > 63 gm 5 wt. %
< 15 [im 10 vol. /0 15-53 gm > 53 gm 5 wt. %
10-45 gm <10 gm 10 vol. % __ > 45 gm 5 wt. %
Table 3 - Examples of Particle size distribution for powder C
PSD Size Max.
< 45 gm 10 wt. %
45-125 gm > 125 nm 10 wt. %
10-53 gm <10 [im 5 wt. %
> 53 gm 5 wt. %
5-30 gm < 5 gm 5 wt. %
> 30 gm 5 wt. %
Process for preparing the powders of the present disclosure
and/or the whole powder bed). This cohesiveness is detrimental to the powder flow properties as more energy is needed to initiate powder avalanches. Because in additive manufacturing operations, the powder needs to be precisely spread out in a uniform fashion at every pass of the operation, such cohesiveness or agglomerate formation caused by the presence of adsorbed water at the surface of the powder particles is, accordingly, highly undesirable.
The atomization method might also use a bar of feedstock molten in passing through an induction coil.
The molten metal then flows towards an atomization nozzle, where streams of high velocity gas disrupt the melt into fine droplets. Another method for atomization uses a rotating electrode contacted by a plasma jet.
The centrifugal force generated by the rotation of the electrode ejects the molten material which then freezes in-flight thus adopting a spherical shape. Another method atomizes molten material from a heated reservoir by spreading the molten material on a rotating disk and subsequent ejection under the centrifugal force generated by the rotation of the disk. The ejected droplets then freeze during freefall thus adopting a spherical shape.
torch to which is made reference above. The particle surface melts and subsequently reshapes into a spherical shape as required for the minimization of Gibbs' free energy. In another contemplated embodiment, the thermal plasma is generated at the exit of a DC plasma torch to which is made reference above or at the apex of the plasma jets generated by a plurality of plasma torches.
Optionally a sheath gas can be provided that protects the walls of the plasma chamber. The sheath gas can also play an active role in the interaction with the powder material.
As the sheath gas is brought in thermal contact with the plasma, it becomes part of the heating media. The hot zone at the apex of the plasma torches can then be expanded on a larger volume to facilitate the interaction with the injected powder cloud.
Prior to step 230, the powder comprises a native oxide outer layer resulting from an oxidation of the outer layer. This layer is also called a pas sivation layer and helps to protect the metal from deeper corrosion. The metal oxide MOx naturally presents OH groups at its surface.
However, the concentration of the hydroxyl group differs from a metal oxide to another and strongly depends on the synthesis method including the gas composition and the water vapor concentration in the powder environment.
surface. Figures 5A to 5C show a non-limiting activation mechanism scheme in the case of a metallic surface in an inert gas plasma, which is in this case, argon. Figure 5A shows the reactive metal surface, which typically has a certain amount of oxygen thereon. As high energy inert gas ions created in the plasma impinge on the surface, they disrupt the electronic structure in the target region which can result, for example, in the breakage of an oxygen bond with the metal, as shown in Figure 5B.
It thus creates surface radicals which are very reactive. If water vapor is present in the vicinity of the activated region and in a sufficiently short timeframe, hydrolysis will occur and -OH moieties will attach to the surface as shown in Figure 5C. Water present at concentrations of about 1000 ppm, or 100 ppm, or even 10 ppm, added intentionally or not, is sufficient in generating hydroxyl groups on the metal surface.
to 6C show a non-limiting possible mechanism responsible for activation in presence of oxygen-containing plasma.
Oxygen radicals as shown in Figure 6A impinge on the metal surface where they form a bond with the metallic substrate, as shown in Figure 6B. Such oxygen atoms remain in a radical state until they encounter water vapor which undergoes hydrolysis to generate -OH groups at the surface, as shown in Figure 6C. The exposure to water vapor can happen either during the plasma process, or out of the plasma reactor, for example, during subsequent steps such as during handling, storage or use.
radiation. Plasmas such as DC and RF plasmas used in plasma atomization produce energetic UV
radiation. These highly energetic photons interact with gaseous oxygen to form ozone, which then react with water vapor to form hydroxyl radicals that are then free to interact with the surface.
SiNR2>SiC1>Si0OCH3>SiOCH3>SiOCH2CH3.
Such a silane with one carbon alkyl chain has the minimum of hydrophobic interactions compared to long chain silanes. This particular alkoxysilane may be advantageous in that it may help to remove the hydrogen bonding between the particles while maintaining the hydrophobic interactions to its lowest. The alkoxy as a leaving group has a low reactivity at room temperature in the absence of a catalyst. Such a situation creates the opportunity of tuning the reaction kinetics through an appropriate choice of catalyst. It is known from research on mesoporous silica that basic catalysis tends to promote condensation at the expense of hydrolysis while the acid catalysis tends to follow the opposite trend.
Consequently, the acid catalysis would promote the formation of oligomers especially in the presence of excess amount of water and the use of basic catalysis would promote the grafting. The basic catalysis precisely meets the goal being sought in tuning the process for the present application.
As hydrolysis begins, condensation becomes possible. Since at the very beginning the probability that a silanol moiety will encounter a hydroxyl from the surface is much greater that the probability of it encountering a second silanol from another silane molecule, the majority of molecules will attach at the surface of the powder. Since the condensation dynamics are highly favored, the equilibrium will remain in favor of attachment at the surface sites rather than between free silanes.
If n is greater than 1, n hydrolyses are possible on each silane molecule. It is therefore possible to attach more molecules to surface bound silanes. In this case, however, steric hindrance and a lower reactivity of the bonds towards hydrolysis make this event less likely than the attachment to a free hydroxyl. As more and more surface hydroxyls become occupied, however, the event becomes more likely.
In practice, the amount of silicon added to a typical laser melting range Ti64 powder will be of about to 100 ppm.
Variants
The fluid is then recirculated in the system with addition of fresh reactants.
The resulting slurry is then dried in a disc dryer, for example.
The example of the powder treatment in a bubbler in fluid connection with the atomizer is a good example where a more dilute suspension is required.
Additive manufacturing process
The powdered material may be sealed inside the storage chamber in a controlled atmosphere such as air, nitrogen, argon, helium, or other inert or noble gas.
When the portion of a powder layer corresponding to the geometry of a two-dimensional slice of a 3D object (part) is fused or bonded together, a next layer of the powdered material is dispensed on the surface of the powder bed to continue the print cycle. The printed part and remaining un-sintered powdered material need to be removed from the build platform when the printing job is finished to allow a next cycle to begin.
laser, NdCrYAG laser, Er:YAG laser, Neodymium YLF (Nd:YLF) solid-state laser, Neodymium doped Yttrium orthovanadate (Nd:YV04) laser, Neodymium doped yttrium calcium oxoborateNd:YCa40 (B03)3 or simply Nd:YCOB, Neodymium glass (Nd:Glass) laser, Titanium sapphire (Ti:sapphire) laser, Thulium YAG (Tm:YAG) laser, Ytterbium YAG (Yb:YAG) laser, Ytterbium:203 (glass or ceramics) laser, Ytterbium doped glass laser (rod, plate/chip, and fiber), Holmium YAG (Ho:YAG) laser, Chromium ZnSe (Cr:ZnSe) laser, Cerium doped lithium strontium (or calcium)aluminum fluoride (Ce:LiSAF, Ce:LiCAF), Promethium 147 doped phosphate glass (147Pm+3:Glass) solid-state laser, Chromium doped chrysoberyl (alexandrite) laser, Erbium doped anderbium-ytterbium co-doped glass lasers, Trivalent uranium doped calcium fluoride (U:CaF2) solid-state laser, Divalent samarium doped calcium fluoride (Sm:CaF2) laser, or F-Center laser.
For instance, in this embodiment, the bed platform 622 may be actuated by an actuator 626 such that it moves relative to the walls 6241-624, and to the chamber 602 towards an elevation axis 628, while the walls 6241-624, do not move relative to the chamber 602. Each movement of the bed platform 622 relative to the walls 6241-624, may typically be for allowing manufacture of a new layer 612' of the three-dimensional metal part 610. As such, after a layer 612 of the three-dimensional metal part 610 is manufactured, as shown in Figure 19, the bed platform 622 may be lowered by the actuator 624 by a dimension TL corresponding to a thickness of a new layer 612' that is to be manufactured (or to the thickness of each layer 612 where the three-dimensional metal part 610 is manufactured with layers of constant thickness), as shown in Figure 20.
of the new layer 646' is constant over its entire surface.
This layer is considered irreversibly bound and remains at the surface even with prolonged heating in an oven. The second layer gains mobility but remains confined by the rigidity of the first layer while the third layer is considered free, and can be removed upon heating at 65 C. However, all three layers are easily recovered when exposed to air at ambient temperatures. In an additive manufacturing apparatus, the powders are likely to be fully hydrated, unless very stringent drying protocols are put in place.
Even then, the first hydration layer will typically remain. When the laser strikes the powder grain, all the adsorbed water suddenly evaporates and is likely to dissociate. This will contribute to the vapor jet that carries highly oxidized metal projections. This absorbed water thus may cause an environment of the additive manufacturing process to be spoiled. Indeed, as the laser encounters adsorbed water, the latter is vaporized and partly dissociates into oxygen and hydrogen elements.
The released oxygen and hydrogen are then free to react with the un-melted powder and the molten (thus highly reactive) material. Oxygen uptake in un-melted powder is typically the main cause why powders have a limited life cycle, i.e., there is a limited number of cycles available before the powders get out of specification due to high levels of oxygen content. Oxygen uptake into the molten material in certain cases will have detrimental effects on final parts, including embrittlement and fatigue resistance.
Having less cohesiveness results in a better density therefore a more reliable melting. The laser power can then be lowered accordingly.
For example, while keeping other parameters constant, the powder 10 may allow a power reduction of the laser 652 of at least 0.5%, in some embodiments of at least 1%, in some embodiments of at least 2%, in some embodiments of at least 5%, in some embodiments of at least 10 /0 and in some embodiments even more.
For instance, in some embodiments, while keeping other parameters constant, the powder 10 may allow the scanning speed of the laser beam 652 to increase by at least 0.5%, in some embodiments of at least 1%, in some embodiments of at least 2%, in some embodiments of at least 5%, in some embodiments of at least 10 /0 and in some embodiments even more.
Metal part
Additionally, the three-dimensional metal part manufactured with the powder of the present disclosure may have a better ultimate tensile strength (UTS) and/or an elongation at break (A%) due to improved characteristics of the powder which in turn reduce the presence of porosities and/or micro-cracks in the body of the metal part.
The specimens built with powders according to the present disclosure showed improvements on the order of 12 to 18 % on the yield strength and on the order of 8 to 13 % on the ultimate tensile strength (See Figures 46A and 46B). The gains were observed in all of the x,y,x=y (w) and z sample directions relative to the build orientation.
may allow the three-dimensional metal 610 to have the herein described characteristics.
Those porosities and/or micro-cracks 38 may alter the structure of the end products. The porosities and/or micro-cracks 38 are, however, significantly diminished (if not absent) from the end-product using the powder 10, as shown in Figure 25B. For instance, in some embodiments the end-product additively manufactured using the powder 10 may be at least 90% porosity-free, in some embodiments at least 95% porosity-free, in some embodiments at least 98% porosity-free, in some embodiments at least 99% porosity-free, and in some embodiments even more (e.g., about 100% porosity-free).
In this embodiment, the three-dimensional metal part 610 manufactured using additive manufacturing with a powder 10 may not need to be machined after being additively manufactured.
flowability, apparent density, PSD, low proportion of aggregate, etc.) allowing reducing thickness TL of the layers 6121-612p and 6461-646L. For instance, in some embodiments, the thickness TL of the layers 6461-646L may be no more than 50 [im, in some embodiments be no more than 40 [im, in some embodiments be no more than 30 [im, in some embodiments be no more than 20 [im, in some embodiments be no more than [im, and in some embodiments even less.
Practical implementations
0.20x the D90 size of the additive manufacturing powder used in the powder bed fusion additive manufacturing process using a laser as a source of thermal energy, which is surprising and unexpected at least because typically one would expect the surface finish to reflect the D90 granulometry of the additive manufacturing powder, in other words one would expect that the irregularities at the surface are substantially of the same size as the D90 size of the powder.
Passive millimeter-wave and THz components are traditionally fabricated by computer numerical control (CNC), micromachining, electrical discharge machining (EDM), or injection molding.
and 0.017 inches [i.e., 0.4318 mm]). In some embodiments, the elongate cavity 720 may have a complex shape such as a "H" shape, as shown in Figures 49 to 51. Other shapes of the elongate cavity 720 may include, for example, a circular shape, as shown in Figures 52 and 59 to 62, a rectangular shape, as shown in Figures 53 to 58, or a square shape, as shown in Figure 61. In some embodiment, the elongate cavity 720 may be relatively long. In some embodiment, the elongate cavity 720 may comprise one, two, three or more bends 736 and/or deviations 738 of at least 5', at least 15 , at least 30 , at least 45 , at least 60 , at least 90 , at least 135', at least 180', at least 360', or even more.
Alternatively, one can use the traditional technique to determine this parameter using a Surface Roughness Testers which use a scanning cantilever in physical contact with the sample to measure the roughness parameter.
Recycling / reusing powders
The powdered material forming the powder bed may be collected in a hopper for reuse in later print jobs. The powder collecting process may be automated, and vacuuming or gas jet systems also used to aid powder dislodgement and removal
In one embodiment, the sensors 742 may comprise a camera and the characteristic of the powder 10 may comprise a visual aspect of an upper surface 746 of the pool 730. In one embodiment, the visual aspect comprises a size and a color of the particles 20.
The processing apparatus 780 may comprise an interface 782, a processing portion 788, and a memory portion 790, which are implemented by suitable hardware and/or software.
processor of the processing portion 788 may be a general-purpose processor executing program code stored in the memory portion 790. Alternatively, a processor of the processing portion 788 may be a specific-purpose processor comprising one or more preprogrammed hardware or firmware elements (e.g., application-specific integrated circuits (ASICs), electrically erasable programmable read-only memories (EEPROMs), etc.) or other related elements.
A memory of the memory portion 790 may be a semiconductor medium (including, e.g., a solid-state memory), a magnetic storage medium, an optical storage medium, and/or any other suitable type of memory. A memory of the memory portion 790 may be read-only memory (ROM) and/or random-access memory (RAM), for example.
Additional improvements to manufacturing process
roll, rake, etc.). In this example, during the recoating step, rather than lowering the three-dimensional metal part 610 between after each layer 646' is fused into a new layer 612' and using the spreading tool 644 to spread a layer 646' of powder 10 over the three-dimensional metal part 610, the three-dimensional metal part 610 may be contained within walls and, after each layer 612 is formed, a pre-determined volume Vp of particles 10 may be incorporated or spread over the three-dimensional metal part 610.
Because the particles 10 are fluid-like, the particles 10 may cover the end-product horizontally, creating a layer 646' of constant thickness. For instance, in some embodiments, as shown in Figure 39 the additive manufacturing 600 may be provided with a vibrating actuator 696 which creates a vibration, providing energy to the powder 10 such that the particles move relative to one another such as to cover the end-product horizontally, creating the layer 646' when vibration of the vibrating actuator 696 ends.
In this embodiment, the powder pool 630 is received in the cavity defined by the walls 6241-624w and the bed 690. In this embodiment, the bottom-up 3D-printer comprises an elevating platform 684 which can be lowered and/or elevated by the actuator 626, and the elevating platform 684 may comprise a surface 693 at an underside of the elevating platform 684 that is configured to interlock with the three-dimensional metal part 610 while the three-dimensional metal part 610 is manufactured. The laser 650 and the scanner 660 may be located at an underside of the powder pool 630. At first, the elevating platform 684 may be positioned such that the surface 693 is at a distance corresponding to the dimension TL from the bed 690. Then the laser beam 650 may pass through the transparent interface 692 of the bed 690 to scan and melt particles of the powder pool 630 disposed in the gap between the bed 690 and the elevating platform 684 such that the molten material adheres to the surface 693 of the elevating platform 684. After a first layer 6121 of the end-product is printed, the actuator 626 may elevate the platform 684 and the first layer 6121 adhered thereto by the dimension TL. An actuator 696, such as a vibrating actuator, may be connected to at least part of the built platform 620 of the bottom-up 3D-printer to create a vibration that will facilitate flow of the particles of the powder pool 630 such that the particles evenly flow in the newly-created gap between the platform 684 and the bed 690. This
In some embodiment, the operator may adapt the settings of the blower 656 to ensure that the blower 656 blows enough air to remove the aggregate, but not too much as this may remove too much powder 10 and create a cloud of powder particles 20 in suspension, which may reduce efficiency of manufacturing. In this example, the operator may input one or more characteristics (e.g., size of the particles 20, flowability, etc.) of the powder 10 that is used to manufacture the three-dimensional metal part 610. In other embodiments, this may be achieved automatically by the manufacturing apparatus 600. For instance, the manufacturing apparatus 600 may comprise sensors to measure a characteristic (e.g., size of the particles 20, flowability, etc.) of the powder 10 and adjust the settings of the blower 656 accordingly. The manufacturing apparatus 600 may also use machine learning algorithms to determine the best working settings for different types of powder, depending on pre-determined characteristics (e.g., size of the particles 20, flowability, etc.).
The interface 912 may be connected to the sensor in the manufacturing apparatus 600 to automatically assess the characteristics 8921-892c and may be further connected to the tools of the manufacturing apparatus 600 to allow the processing apparatus 880 to control them.
Controlling the atmosphere
However, some of these cross-flow solutions cause undesirable gas flow structures (e.g., stagnation, recirculation of gas within the enclosure that may lead to a steady state) that do not completely solve the debris related issues. It may be desirable to establish a gas flow solution that avoids the undesirable gas flow structures and allows removal of debris from the enclosure atmosphere. At times, during the 3D
printing, various material forms become gas-borne. The material forms may compromise (e.g., fine) powder or soot. Some of the gas-borne material may be susceptible to reaction with a reactive agent (e.g., an oxidizing agent). Some of the gas-borne material may violently react (e.g., when coming into contact with the reactive agent). At times, it may be desirable to provide low leakage of the reactive agent (e.g., oxygen in the ambient atmosphere) into one or more segments of the 3D printer. At times, it may be desirable to isolate the interior of one or more segments of the 3D printer from a harmful (e.g., violently reactive) level of the reactive agent (e.g., that is present in the atmosphere external to the one or more segments of the 3D printer). At times, it may be desirable to preserve a non-reactive (e.g., inert) atmosphere in at least one segment of the 3D
printer (e.g., before, during and/or after the 3D printing).
It may be desirable to incorporate a filter mechanism that is separated (e.g., isolated) from an external (e.g., ambient) atmosphere comprising the reactive agent. It may be desirable to incorporate a filter mechanism that maintains an inert interior atmosphere around the filter, at least during the filtering operation and/or disassembling of the filter from the filtering mechanism. It may further be desirable to facilitate an uninterrupted exchange of the filter in the filtering mechanism, for example, in order to facilitate continuous separation of gas-borne material from the recirculating gas in at least one or more segments of the 3D printer during the 3D printing, for example, when the filter clogs and requires exchange and/or refurbishing.
Variants
Tests
Angle of repose /Hall flowmeter
Avalanche angle
ASTM Ell meshes sieving
Surface roughness
Other ASTM Standards
(Extra Low Interstitial) Alloy for Surgical Implant Applications (UNS R56401)
designates nanometers.
defines the relative amount of particles present according to size. The most easily understood method of determination is sieve analysis, where powder is separated on sieves of different sizes.
Thus, the PSD is defined in terms of discrete size ranges: e.g. a PSD of between 45 [im and 53 [1m, when sieves of these sizes are used. The PSD is usually determined over a list of size ranges that covers nearly all the sizes present in the sample.
generally refers to a powder which has not been surface modified (for example, a powder which has been atomized and optionally sieved).
EXAMPLES
Example 1
relative humidity.
4.05 g methyltrimethoxysilane was then dissolved into 400 ml ethanol (95%, denatured) (sol. 2). A third solution contained only the ethanol solution (95%, denatured) (sol. 3). The V-blender rotation was activated and the injection mechanism through intensifier bars was activated.
The solutions were then injected sequentially: sol 1, then sol 2, then sol 3. The vessel was then pressurized and closed airtight. The mixture was allowed to react for 4 hours, at which point a 12 standard liter per minute (slpm) argon gas flow was established through the vessel and the temperature was raised at 50 C
for drying. The mixture was left to dry for 4 hours with rotation of the mixer. The powder was then transferred to a canister and sieved.
and Hall flow results varying by less than 3 seconds, or 7%, between 10 /0 of relative humidity and 75% of relative humidity.
Example 2
Table 4 Metal powder Solvent Silane Ti64, AlSi10Mg, Toluene, hexane, heptane, Methyl trimethoxysilane, Methyl AlSi7Mg, Ni718 cyclohexane, decane, triethoxysilane, dodecane, tetradecane. dimethyldiethoxysilane, dimethyldimethoxysilane, Vinyltrimethoxysilane, phenyltrimethoxysilane, diphenyldimethoxysilane.
Example 3
of coupling agent was added (Di-(2-ethylhexyl)phosphoric acid or Oleic acid or sodium dodecyl sulfate), and the suspension was heated at 50 C for 4 h. The mixture was vacuum filtered with a Buchner, washed with ethanol followed by a drying step. Figure 1 shows the hydrophobic character of the powder 10 after the treatment in that water added to the powder forms a cohesive droplet 35 on top of the powder.
Example 4
B213 from 10% relative humidity up to 75% relative humidity.
for drying. The mixture was left to dry for 2 hours with rotation of the mixer. The powder was then transferred to a canister and sieved. As shown in Figure 13, the flowability curve obtained according to ASTM B213 indicates: Hall flow results decreasing (i.e. signifying an increasing flowability) as relative humidity increases; Hall flow results being less than 34 seconds; and Hall flow results varying by less than 14 seconds, or 42%, between 10% of relative humidity and 75% of relative humidity.
Example 5
B213 from 10% relative humidity up to 75% relative humidity.
The powder was then transferred to a canister and sieved. As shown in Figure 14, the flowability curve obtained according to ASTM B213 indicates: Hall flow results generally decreasing (i.e.
signifying an increasing flowability) as relative humidity increases; Hall flow results being less than 27 seconds; and Hall flow results varying by less than 5 seconds, or 19%, between 10% of relative humidity and 75% of relative humidity.
Example 6
B213 from 10% relative humidity up to 75% relative humidity.
signifying an increasing flowability) as relative humidity increases; Hall flow results being less than 25 seconds; and Hall flow results varying by less than 3 seconds, or 11%, between 10 /0 of relative humidity and 75% of relative humidity.
Example 7
B213 from 10% relative humidity up to 75% relative humidity.
3 solutions were prepared. First 9 g ammonium hydroxide (30% aqueous) was dissolved into 50 ml ethanol (95%, denatured) (sol. 1). 2.9 g methyltrimethoxysilane was then dissolved into 50 ml ethanol (95%, denatured) (sol. 2). A third solution contained only the ethanol solution (sol. 3, 50 mL). The solutions were then injected sequentially: sol 1, then sol 2, then sol 3. The vessel was then pressurized and closed airtight. The mixture was allowed to react for 1 hour, at which point a 12 slpm argon gas flow was established through the vessel and the temperature was raised at 50 C for drying. The mixture was left to dry for 2 hours with rotation of the mixer. The powder was then transferred to a canister and re-sieved. As shown in Figure 16, the flowability curve obtained according to ASTM
B213 indicates: Hall flow results generally decreasing (i.e. signifying an increasing flowability) as relative humidity increases; Hall flow results being less than 33 seconds; and Hall flow results varying by less than 5 seconds, or 15%, between 10% of relative humidity and 75% of relative humidity.
Example 8
Example 9
relative humidity and the Hall flow results vary by less than 3 seconds, or 7%, between 10% of relative humidity and 75% of relative humidity.
The ammonium hydroxide solution was first added to the container and the contents were thoroughly mixed.
Hall flow results generally stable (i.e. signifying an increasing flowability); Hall flow results being less than 43 seconds; and Hall flow results varying by less than 2 seconds, or 5%, between 10 /0 of relative humidity and 75% of relative humidity.
Example 10
relative humidity.
Methyltrimethoxysilane (0.053 g) was dissolved into ethanol (12.5 ml) and aqueous ammonium hydroxide (30%, 0.15 ml) was mixed with ethanol (12.5 ml) in a second container. The ammonium hydroxide solution was first added to the container and the contents were thoroughly mixed. The silane solution was then added into the container and the contents of the container were thoroughly mixed. The container was placed in a rotating mixer. The mixer was then rotated at 0.5 RPM for 4 hours. As shown in Figure 18, the flowability curve obtained according to ASTM
B213 indicates:
Hall flow results being less than 14 seconds; and Hall flow results varying by less than 3 seconds, or 21%, between 10% of relative humidity and 75% of relative humidity.
to 120 g/L.
to about 250 C, from about 60 C to about 250 C, from about 20 C to about 200 C, from about 30 C to about 200 C, from about 40 C to about 200 C, from about 50 C to about 200 C, from about 60 C to about 200 C, from about 20 C to about 150 C, from about 30 C to about 150 C, from about 40 C to about 150 C, from about 50 C to about 150 C, from about 60 C to about 150 C, from about 20 C to about 100 C, from about 30 C to about 100 C, from about 40 C to about 100 C, from about 50 C to about 100 C, from about 60 C to about 100 C, or any temperature within these ranges.
Moreover, certain theories may be proposed and disclosed herein; however, in no way they, whether they are right or wrong, should limit the scope of the invention so long as the invention is practiced according to the present disclosure without regard for any particular theory or scheme of action.
"containing," or "characterized by," is inclusive or open-ended and does not exclude additional, un-recited elements or method steps.
In the case of conflict, the present document, including definitions will control.
Claims (501)
including a fraction of fine particles having a size 20 pm in a quantity of up to 30 vol%, and the powder having a flowability of 40s determined in accordance with ASTM B213 at 30%
relative humidity.
including a fraction of fine particles having a size 20 m in a quantity of up to 30 vol%, and the powder having a measurable flowability determined in accordance with ASTM B213 at 75% relative humidity.
relative humidity.
relative humidity.
relative humidity, wherein the second apparent density represents a loss of 2% relative to the first apparent density.
B213 at 75% relative humidity.
125.
125.
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| KR20220019680A (en) | 2019-05-02 | 2022-02-17 | 테크나 플라즈마 시스템 인코포레이티드 | Additive manufacturing powder with improved physical properties, manufacturing method and use thereof |
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2020
- 2020-05-01 KR KR1020217038679A patent/KR20220019680A/en not_active Abandoned
- 2020-05-01 CN CN202080041043.8A patent/CN113924177B/en active Active
- 2020-05-01 JP JP2021564797A patent/JP7707077B2/en active Active
- 2020-05-01 CA CA3138388A patent/CA3138388A1/en active Pending
- 2020-05-01 CN CN202410891558.7A patent/CN118905220A/en active Pending
- 2020-05-01 WO PCT/CA2020/050590 patent/WO2020220143A1/en not_active Ceased
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- 2020-05-01 US US17/608,398 patent/US12521789B2/en active Active
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP4491300A1 (en) | 2023-06-29 | 2025-01-15 | General Electric Company | System and method for atomized powder processing and a processed powder |
Also Published As
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| CN113924177A (en) | 2022-01-11 |
| AU2020266480A1 (en) | 2021-12-23 |
| EP3962677A4 (en) | 2023-01-04 |
| CN113924177B (en) | 2024-07-02 |
| KR20220019680A (en) | 2022-02-17 |
| AU2020266480B2 (en) | 2026-03-12 |
| EP3962677A1 (en) | 2022-03-09 |
| JP7707077B2 (en) | 2025-07-14 |
| JP2022530984A (en) | 2022-07-05 |
| US20220288676A1 (en) | 2022-09-15 |
| WO2020220143A1 (en) | 2020-11-05 |
| US12521789B2 (en) | 2026-01-13 |
| CN118905220A (en) | 2024-11-08 |
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