US20090047165A1 - Metal powder for use in an additive method for the production of three-dimensional objects and method using such metal powder - Google Patents
Metal powder for use in an additive method for the production of three-dimensional objects and method using such metal powder Download PDFInfo
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- US20090047165A1 US20090047165A1 US12/152,452 US15245208A US2009047165A1 US 20090047165 A1 US20090047165 A1 US 20090047165A1 US 15245208 A US15245208 A US 15245208A US 2009047165 A1 US2009047165 A1 US 2009047165A1
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- 239000000843 powder Substances 0.000 title claims abstract description 152
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 54
- 239000002184 metal Substances 0.000 title claims abstract description 54
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 31
- 239000000654 additive Substances 0.000 title claims abstract description 25
- 230000000996 additive effect Effects 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims description 56
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002245 particle Substances 0.000 claims abstract description 26
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000010894 electron beam technology Methods 0.000 claims abstract description 13
- 229910052742 iron Inorganic materials 0.000 claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 10
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 10
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 10
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 10
- 239000011651 chromium Substances 0.000 claims abstract description 10
- 229910052802 copper Inorganic materials 0.000 claims abstract description 10
- 239000010949 copper Substances 0.000 claims abstract description 10
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 239000000203 mixture Substances 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 12
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 9
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 9
- 229910052748 manganese Inorganic materials 0.000 claims description 9
- 239000011572 manganese Substances 0.000 claims description 9
- 229910052750 molybdenum Inorganic materials 0.000 claims description 9
- 239000011733 molybdenum Substances 0.000 claims description 9
- 229910052758 niobium Inorganic materials 0.000 claims description 9
- 239000010955 niobium Substances 0.000 claims description 9
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 claims description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 8
- 229910052698 phosphorus Inorganic materials 0.000 claims description 8
- 239000011574 phosphorus Substances 0.000 claims description 8
- 229910052717 sulfur Inorganic materials 0.000 claims description 8
- 239000011593 sulfur Substances 0.000 claims description 8
- 238000009826 distribution Methods 0.000 claims description 6
- 229910000734 martensite Inorganic materials 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 238000000889 atomisation Methods 0.000 claims description 4
- 229910000859 α-Fe Inorganic materials 0.000 claims description 4
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 238000000149 argon plasma sintering Methods 0.000 description 23
- 229910001220 stainless steel Inorganic materials 0.000 description 13
- 239000010935 stainless steel Substances 0.000 description 13
- 239000000463 material Substances 0.000 description 10
- 238000010438 heat treatment Methods 0.000 description 9
- 238000004881 precipitation hardening Methods 0.000 description 6
- 238000000137 annealing Methods 0.000 description 5
- 238000009864 tensile test Methods 0.000 description 5
- 238000011282 treatment Methods 0.000 description 5
- 238000010791 quenching Methods 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 230000000171 quenching effect Effects 0.000 description 3
- 230000032683 aging Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005275 alloying Methods 0.000 description 1
- 229910001566 austenite Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 238000009689 gas atomisation Methods 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000004372 laser cladding Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000003913 materials processing Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 239000012768 molten material Substances 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000009692 water atomization Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C33/00—Making ferrous alloys
- C22C33/02—Making ferrous alloys by powder metallurgy
- C22C33/0257—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements
- C22C33/0278—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5%
- C22C33/0285—Making ferrous alloys by powder metallurgy characterised by the range of the alloying elements with at least one alloying element having a minimum content above 5% with Cr, Co, or Ni having a minimum content higher than 5%
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/20—Direct sintering or melting
- B22F10/28—Powder bed fusion, e.g. selective laser melting [SLM] or electron beam melting [EBM]
-
- 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
- B22F3/105—Sintering only by using electric current other than for infrared radiant energy, laser radiation or plasma ; by ultrasonic bonding
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F10/00—Additive manufacturing of workpieces or articles from metallic powder
- B22F10/60—Treatment of workpieces or articles after build-up
- B22F10/64—Treatment of workpieces or articles after build-up by thermal means
-
- 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
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
-
- 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 relates to a metal powder for use in an additive method for the production of three-dimensional objects and to a method using such a powder.
- Direct Metal Laser Sintering is a laser-based rapid prototyping and tooling process by means of which net shape parts are fabricated in a single process. Complex parts can be directly produced from 3D-CAD models by layer-wise solidification of metal powder layers in portions of the layer corresponding to the cross-section of the three-dimensional part in the respective layer. This process is described in detail for example in Juha Kotila et al., Steel-based Metal Powder Blend for Direct Metal Laser Sintering Process, Advances in Powder Metallurgy & Particular Materials—1999, Vol. 2 Part 5, p. 87-93 and in T. Syvanen et al., New Innovations in Direct Metal Laser Sintering Process—A Step Forward in Rapid Prototyping and Manufacturing, Laser Materials Processing, Vol. 87, 1999, p. 68 to 76.
- the object should be able to undergo the precipitation hardening process to fulfill the requirements of users.
- a method for producing a three-dimensional object shall be provided.
- a metal powder for use in an additive production method of three-dimensional objects wherein the powder is solidified by means of a laser or electron beam or another heat source.
- the metal powder is characterized in that the powder comprises iron and the following components by weight percent (wt.-%)
- the metal powder of the present invention also can comprise one or more of the following features:
- a metal powder in accord with the invention comprises:
- a metal powder in accord with the invention comprises iron and the following components by weight percent (wt.-%):
- the present invention provides a method for the production of three-dimensional objects from a powder, wherein the powder is applied in an additive manner and is solidified by means of a laser or electron beam or another heat source, characterized in that the powder used is a powder as described herein.
- Methods for the production of three-dimensional objects from a powder also can comprise one or more of the following features:
- the invention also provides three-dimensional objects produced by the methods as described herein.
- the metal powder according to the invention has the advantage that the object produced can be post-hardened, in particular by means of precipitation hardening, to significantly increase the hardness. Furthermore, the mechanical properties of the three-dimensional object produced by an additive manufacturing method are similar to those achieved using conventional 17-4 PH stainless steel and a conventional manufacturing method. This opens a wide range of applications for laser sintering and other additive processes.
- FIG. 1 is a schematic representation of a laser sintering apparatus
- FIG. 2 is a schematic presentation of laser scanning in the DLMS-process
- FIG. 3 a )- 3 c graphs showing the result of typical tensile testing behaviour of parts produced using the metal powder according to the invention.
- FIG. 4 shows yield and ultimate tensile strength results of parts produced using the metal powder according to the invention with different heat treatment cycles.
- the laser sintering apparatus comprises a build container 1 open at the top with a support 2 carrying the object 3 to be built.
- the support 2 is movable in the build container 1 in a vertical direction and is adjusted in such a way that the layer of the object which is to be solidified defines a working plane 4 .
- a layer generating device 5 for generating a layer of pulverulent build material on the support or on a previously applied layer is provided.
- the laser sintering apparatus further comprises a laser 6 emitting a laser beam 7 which is deflected by a deflection unit 8 and passes through an optical unit 10 which focuses the laser beam onto the working plane 4 .
- a control unit 9 controls the deflection unit 8 and the optical unit 10 in such a way that the laser beam 7 can be focussed to any position in the working plane.
- a powder reservoir and feeding device 11 is provided which is, in the example shown, arranged above the build container and which contains the pulverulent build material and feeds it to the layer generating device 5 .
- the pulverulent build material is a metal powder, preferably a stainless steel powder.
- the powder is produced in a known manner. Preferably it is produced by means of an atomization process, for example gas atomization, wherein the molten material undergoes atomization using gases. However, other processes may also be used, for example water atomization.
- each powder particle has the same or at least a similar chemical composition.
- the components can be pre-alloyed.
- the powder particles have spherical or approximately spherical shape with an aspect ratio up to 1:2.
- the grain size distribution of the powder particles according to the invention is between 0.1 ⁇ m and 125 ⁇ m, the median size expressed as d50 value is between 20 ⁇ m and 100 ⁇ m, preferably between 30 ⁇ m and 50 ⁇ m.
- the metal powder according to the invention comprises iron and the following components given in weight percent (wt.-%):
- the powder comprises in addition 1.00 max. wt.-% of manganese and/or 0.03 max. wt.-% of phosphorus and/or 0.015 max. wt.-% of sulfur and/or 1.0 max. wt.-% of silicon and/or niobium between 0.15 and 0.45 wt.-% and/or 0.5 max. wt.-% of molybdenum and/or 0.10 max. wt.-% of nitrogen.
- the nitrogen has significant influence on metallurgical phases and can change the metallurgical phase from martensitic to austenitic or semi-austenitic.
- the balance of the composition is iron.
- the powder is completely free of or nearly free of ferrite with a ferrite content of less than 5 wt.-%.
- the powder is a purely metal powder without non-metallic additives such as fluxing agents etc.
- the powder according to the invention comprises the following components in weight percent (wt.-%):
- the median particle size (d50) of the more preferred example is between 30 ⁇ m and 40 ⁇ m.
- the method according to the invention is explained with reference to FIGS. 1 and 2 using laser sintering as an additive process for manufacturing the object 3 .
- the data of the 3D-CAD model of the object 3 to be built are converted in a known manner and transferred to the computer of the laser sintering apparatus for controlling the laser sintering apparatus during the sintering process.
- the powder according to the invention is dispensed onto the support or a previous layer and thereafter sintered or melted in each layer at locations corresponding to the cross-section of the object 3 .
- the focused laser beam spot size at the powder melting level is between 20 ⁇ m and 500 ⁇ m, preferably approximately 120 ⁇ m.
- the laser scanning velocity is between 50 mm/s and 10000 mm/s, preferably approximately 1000 mm/s and the distance between adjacent scan lines is between 0.02 mm and 0.5 mm, preferably approximately 0.1 mm.
- the thickness of the powder layer is between 10 ⁇ m and 200 ⁇ m preferably approximately 20 ⁇ m.
- An inert gas flow may be used to avoid chemical reaction of the powder with surrounding material or air.
- the laser beam scans the surface of the metal powder layer.
- the high intensity laser radiation is absorbed by the powder particles and creates extremely rapid heating in the powder to melt the powder.
- heat is conducted away from the previously melted area via the solid metal and/or metal powder under and/or around it, leading to rapid cooling and resolidification.
- Active cooling can be carried out for example by means of cooling the support platform or by means of a flow of cooled gas.
- the laser sintered object is a stainless steel object having less than 20% of the austenitic phase.
- the object 3 is post-treated.
- Heat treatment can be carried out at a variety of temperatures to develop specific properties.
- the eight standard heat treatments H900, H925, H1025, H1075, H1100, H1150, H1150+1150, H1150-M can be carried out.
- solution annealing (SA) can be carried out to obtain desired properties. It has been observed that high cooling rates to a relatively low temperature during laser processing are essential in order to obtain a complete martensitic transformation and to avoid excess amount of remaining austenite phase in the resolidified metal. This is important for the subsequent post-treatments like H900, H925, H1025, etc. if the treatments are to be done without solution annealing and quenching. If the cooling rate is not sufficient and the martensitic transformation is only partial then additional solution annealing and subsequent quench is needed to obtain a fully martensitic phase structure which is more favourable for post-hardening treatments like H900, H925.
- the method according to the invention has the additional advantage that by carrying out the laser processing with rapid cooling and resolidification, additional steps of post-treatment such as solution annealing and quenching can be omitted. Hence, the process chain becomes shorter.
- FIG. 3 a ) to 3 c ) show a typical tensile testing behaviour of a laser sintered specimen.
- the tensile testing behaviour has been tested with a 3.56 mm thick flat test specimen according to MPIF 10 standard.
- FIG. 3 a shows the result for a specimen produced using known stainless steel powder 17-4 PH.
- FIG. 3 b shows a typical tensile testing behaviour of specimens produced using the metal powder according to the above described more preferred embodiment of the invention.
- C 1 , C 2 and C 3 are measurement results from three specimens manufactured under the same conditions, i.e. identical process parameters and geometries.
- FIG. 3 c shows a typical tensile testing behaviour of specimens which are aged according to H900 condition after laser sintering.
- D 1 , D 2 and D 3 are measurement results of three specimens with the same process parameters and the same H900 heat treatment condition.
- the object produced using the metal powder according to the invention has considerably higher strength than the object which is produced using known stainless steel powder. Strength can be enhanced further by using heat treatment.
- FIG. 4 shows the yield and ultimate tensile strength of objects produced by laser sintering using the metal powder according to the above preferred embodiment wherein the object underwent various heat treatment conditions, respectively. As can be seen, the precipitation hardening is applicable.
- HV1 is the hardness in Vickers units using 1 kg load for testing; HRC is the hardness in Rockwell C scale.
- the objects produced with laser sintering and using the metal powder according to the invention are stronger, stiffer and harder than that produced using the powder according to the prior art.
- a heat treatment comprising ageing at 482° C. for one hour and air cooling provides superior mechanical properties due to precipitation hardening. Solution annealing and quenching is not required before the ageing treatment.
- the metal powder according to the invention is not limited to the examples described above.
- the metal powder can be a blend of different component powders.
- the blend of component powders has to be selected such that the resulting powder mixture has in total a chemical composition and grain size distribution identical or similar to the powder embodiments described above.
- the individual component powders in the blend can differ in grain size and/or in chemistry. When they differ in chemical composition, the alloying to the final stoichiometry takes place during the laser sintering process.
- the metal powder is a blend of different component powders each having the above composition but which have different particle size distributions. Such blends can be beneficial for fine tuning the chemical composition and the grain size distribution of the resulting blended powder.
- the invention is not limited in the application to the laser sintering technique. Moreover, electron beam sintering or melting or mask sintering using a spacious heat source can also be used.
- the invention is not even limited to additive layer-wise production methods but includes other additive and free-form production methods of three-dimensional objects such as, for example, the 3D laser-cladding method.
Abstract
A metal powder for use in an additive production method of three-dimensional objects is disclosed. The powder is solidified by means of a laser or electron beam or another heat source and contains iron and the following components by weight percent (wt.-%):
-
- carbon: 0.07 max. wt-%,
- chromium: 14.00-15.50 wt.-%,
- nickel: 3.5-5.0 wt.-%, and
- copper: 3.0-4.5 wt.-%.
The powder particles have a median particle size d50 between 20 μm and 100 μm.
Description
- (1) Field of the Invention
- The invention relates to a metal powder for use in an additive method for the production of three-dimensional objects and to a method using such a powder.
- (2) Description of Related Art
- Direct Metal Laser Sintering (DMLS) is a laser-based rapid prototyping and tooling process by means of which net shape parts are fabricated in a single process. Complex parts can be directly produced from 3D-CAD models by layer-wise solidification of metal powder layers in portions of the layer corresponding to the cross-section of the three-dimensional part in the respective layer. This process is described in detail for example in Juha Kotila et al., Steel-based Metal Powder Blend for Direct Metal Laser Sintering Process, Advances in Powder Metallurgy & Particular Materials—1999, Vol. 2 Part 5, p. 87-93 and in T. Syvanen et al., New Innovations in Direct Metal Laser Sintering Process—A Step Forward in Rapid Prototyping and Manufacturing, Laser Materials Processing, Vol. 87, 1999, p. 68 to 76.
- There is a high demand for processing metal materials by additive manufacturing processes such as Direct Metal Laser Sintering, so that rapid manufacturing can be applied to applications where a specific material having well-known properties is required. One important class of materials is stainless steel which is widely used in many products. Many different kinds of stainless steel exist and are commercially available for conventional manufacturing methods, such as casting, forging, machining etc. as referenced in international standards, reference books, manufacturers' catalogues etc.
- One example of a well-known conventional stainless steel is 17-4 PH (US designation) corresponding to 1.4542 European designation. An important characteristic of this material in conventional use is that it can be post-hardened by precipitation hardening (“PH”) to significantly increase the hardness. This material in powdered form can be processed by laser sintering to produce metal parts with good quality. Depending on how the parameters which are used in this process are selected, different metallurgical phases can be produced. It has been found that the conventional precipitation hardening process does not work for parts produced by direct metal laser sintering using powder material corresponding to stainless steel 17-4PH and typical processing parameters known from the prior art.
- 316 L/1.4404 stainless steel has also been used for laser sintering or laser melting.
- It is the object of the invention to provide a metal powder which can be processed by laser sintering or similar additive manufacturing methods using a heat source and whereby the object produced has similar properties compared to that of a stainless steel object produced using a conventional manufacturing method. In particular, the object should be able to undergo the precipitation hardening process to fulfill the requirements of users. Furthermore, a method for producing a three-dimensional object shall be provided.
- In accord with the present invention, a metal powder is provided for use in an additive production method of three-dimensional objects wherein the powder is solidified by means of a laser or electron beam or another heat source. The metal powder is characterized in that the powder comprises iron and the following components by weight percent (wt.-%)
-
- carbon: 0.07 max. wt-%,
- chromium: 14.00-15.50 wt.-%,
- nickel: 3.5-5.0 wt.-%, and
- copper: 3.0-4.5 wt.-%.
and wherein the powder particles have a median particle size d50 between 20 μm and 100 μm.
- The metal powder of the present invention also can comprise one or more of the following features:
-
- a. the powder particles have an approximately spherical shape;
- b. the powder is produced by atomization;
- c. the component elements are contained in each powder particle in a pre-alloyed manner;
- d. the powder is a blend of different component powders having different grain size distributions and/or chemical compositions;
- e. the powder comprises 1.00 max. wt.-% of manganese;
- f. the powder comprises 0.03 max. wt.-% of phosphorus;
- g. the powder comprises 0.015 max. wt.-% of sulfur;
- h. the powder comprises 1.00 max. wt.-% of silicon;
- i. the powder comprises 0.5 max. wt.-% of molybdenum;
- j. the powder comprises between 0.15 and 0.45 wt.-% niobium;
- k. the powder comprises 0.10 max. wt.-% nitrogen;
- l. the content of ferrite is less than 5 wt.-%; and/or
- m. the powder is in the martensitic state.
- In another embodiment, a metal powder in accord with the invention comprises:
-
- carbon: 0.02 (max. 0.04) wt.-%,
- phosphorus: 0.01 (max. 0.02) wt.-%,
- silicon: 0.4 (max. 0.6) wt.-%,
- nickel: 4.2±0.2 wt.-%,
- copper: 3.6±0.2 wt.-%,
- manganese: 0.1 (max. 0.2) wt.-%,
- sulfur: 0.01 (max. 0.01) wt.-%,
- chromium: 14.3±0.2 wt.-%,
- molybdenum: 0.0 (max. 0.2) wt.-%,
- niobium: 0.3±0.05 wt.-%,
- nitrogen: 0.04 (max. 0.08) wt.-%, and
- iron: balance.
- In still another embodiment, a metal powder in accord with the invention comprises iron and the following components by weight percent (wt.-%):
-
- carbon: 0.02 to 0.04 wt.-%,
- phosphorus: max. 0.02 wt.-%,
- silicon: 0.4 to 0.6 wt.-%,
- nickel: 4.2±0.2 wt.-%,
- copper: 3.6±0.2 wt.-%,
- manganese: max. 0.2 wt.-%,
- sulfur: max. 0.01 wt.-%,
- chromium: 14.3±0.2 wt.-%,
- molybdenum: max. 0.2 wt.-%,
- niobium: 0.3±0.05 wt.-%,
- nitrogen: max. 0.08 wt.-%, and
- iron: balance.
- Also, the present invention provides a method for the production of three-dimensional objects from a powder, wherein the powder is applied in an additive manner and is solidified by means of a laser or electron beam or another heat source, characterized in that the powder used is a powder as described herein.
- Methods for the production of three-dimensional objects from a powder, in accord with the invention, also can comprise one or more of the following features:
-
- i. the powder is applied in a layer-wise manner and selectively solidified in each layer at locations corresponding to the cross-section of the three-dimensional object;
- ii. a laser beam is used with a laser power between 20 W and 1 kW, preferably approximately 200 W;
- iii. the focused laser beam spot size at the powder melting level is between 20 μm and 500 μm, preferably approximately 120 μm;
- iv. the laser scanning velocity is between 50 mm/s and 10000 mm/s, preferably approximately 1000 mm/s;
- v. the distance between adjacent scan lines is between 0.02 and 0.5 mm, preferably approximately 0.1 mm;
- vi. the thickness of the powder layer is between 10 μm and 200 μm, preferably approximately 20 μm;
- vii. the three-dimensional object is precipitation hardened after the layer-wise formation;
- viii. a step of cooling during the additive production method; and/or
- ix. the process parameters are selected such that the object comprises less than approximately 20% of the austenitic phase.
- In addition, the invention also provides three-dimensional objects produced by the methods as described herein.
- The metal powder according to the invention has the advantage that the object produced can be post-hardened, in particular by means of precipitation hardening, to significantly increase the hardness. Furthermore, the mechanical properties of the three-dimensional object produced by an additive manufacturing method are similar to those achieved using conventional 17-4 PH stainless steel and a conventional manufacturing method. This opens a wide range of applications for laser sintering and other additive processes.
- Further advantages of the invention will become apparent from the description of embodiments in conjunction with the accompanying drawings, wherein:
-
FIG. 1 is a schematic representation of a laser sintering apparatus, -
FIG. 2 is a schematic presentation of laser scanning in the DLMS-process, -
FIG. 3 a)-3 c) graphs showing the result of typical tensile testing behaviour of parts produced using the metal powder according to the invention, and -
FIG. 4 shows yield and ultimate tensile strength results of parts produced using the metal powder according to the invention with different heat treatment cycles. - The invention will now be described with reference to the direct metal laser sintering process as an example for an additive manufacturing method. As shown in
FIG. 1 the laser sintering apparatus comprises a build container 1 open at the top with asupport 2 carrying theobject 3 to be built. Thesupport 2 is movable in the build container 1 in a vertical direction and is adjusted in such a way that the layer of the object which is to be solidified defines a workingplane 4. A layer generating device 5 for generating a layer of pulverulent build material on the support or on a previously applied layer is provided. The laser sintering apparatus further comprises alaser 6 emitting alaser beam 7 which is deflected by adeflection unit 8 and passes through anoptical unit 10 which focuses the laser beam onto the workingplane 4. Acontrol unit 9 controls thedeflection unit 8 and theoptical unit 10 in such a way that thelaser beam 7 can be focussed to any position in the working plane. A powder reservoir and feedingdevice 11 is provided which is, in the example shown, arranged above the build container and which contains the pulverulent build material and feeds it to the layer generating device 5. - According to the invention, the pulverulent build material is a metal powder, preferably a stainless steel powder. The powder is produced in a known manner. Preferably it is produced by means of an atomization process, for example gas atomization, wherein the molten material undergoes atomization using gases. However, other processes may also be used, for example water atomization. As a result of the production process, each powder particle has the same or at least a similar chemical composition. The components can be pre-alloyed. In addition, the powder particles have spherical or approximately spherical shape with an aspect ratio up to 1:2.
- The grain size distribution of the powder particles according to the invention is between 0.1 μm and 125 μm, the median size expressed as d50 value is between 20 μm and 100 μm, preferably between 30 μm and 50 μm.
- The metal powder according to the invention, comprises iron and the following components given in weight percent (wt.-%):
-
- carbon: 0.07 max. wt-%,
- chromium: 14.00-15.50 wt.-%,
- nickel: 3.5-5.0 wt.-%, and
- copper 3.0-4.5 wt.-%
- In a preferred embodiment, the powder comprises in addition 1.00 max. wt.-% of manganese and/or 0.03 max. wt.-% of phosphorus and/or 0.015 max. wt.-% of sulfur and/or 1.0 max. wt.-% of silicon and/or niobium between 0.15 and 0.45 wt.-% and/or 0.5 max. wt.-% of molybdenum and/or 0.10 max. wt.-% of nitrogen. The nitrogen has significant influence on metallurgical phases and can change the metallurgical phase from martensitic to austenitic or semi-austenitic. The balance of the composition is iron.
- Advantageously the powder is completely free of or nearly free of ferrite with a ferrite content of less than 5 wt.-%.
- The powder is a purely metal powder without non-metallic additives such as fluxing agents etc.
- In a more preferred embodiment, the powder according to the invention comprises the following components in weight percent (wt.-%):
-
- carbon: 0.02 (max. 0.04) wt.-%,
- phosphorus: 0.01 (max. 0.02) wt.-%,
- silicon: 0.4 (max. 0.6) wt.-%,
- nickel: 4.2±0.2 wt.-%,
- copper: 3.6±0.2 wt.-%,
- manganese: 0.1 (max. 0.2) wt.-%,
- sulfur: 0.01 (max. 0.01) wt.-%,
- chromium: 14.3±0.2 wt.-%,
- molybdenum: 0.0 (max. 0.2) wt.-%,
- niobium: 0.30±0.05 wt.-%,
- nitrogen: 0.04 (max. 0.08) wt.-%, and
- iron: balance.
- The median particle size (d50) of the more preferred example is between 30 μm and 40 μm.
- The method according to the invention is explained with reference to
FIGS. 1 and 2 using laser sintering as an additive process for manufacturing theobject 3. The data of the 3D-CAD model of theobject 3 to be built are converted in a known manner and transferred to the computer of the laser sintering apparatus for controlling the laser sintering apparatus during the sintering process. The powder according to the invention is dispensed onto the support or a previous layer and thereafter sintered or melted in each layer at locations corresponding to the cross-section of theobject 3. - A laser with a power between 20 W and 1 kW, preferably approximately 200 W, is used. The focused laser beam spot size at the powder melting level is between 20 μm and 500 μm, preferably approximately 120 μm. The laser scanning velocity is between 50 mm/s and 10000 mm/s, preferably approximately 1000 mm/s and the distance between adjacent scan lines is between 0.02 mm and 0.5 mm, preferably approximately 0.1 mm. The thickness of the powder layer is between 10 μm and 200 μm preferably approximately 20 μm. These parameters are selected depending on the ranges depending on the object to be built.
- An inert gas flow may be used to avoid chemical reaction of the powder with surrounding material or air. During the sintering process the laser beam scans the surface of the metal powder layer. The high intensity laser radiation is absorbed by the powder particles and creates extremely rapid heating in the powder to melt the powder. As the scanned laser beam moves on, heat is conducted away from the previously melted area via the solid metal and/or metal powder under and/or around it, leading to rapid cooling and resolidification. By keeping the temperature of the process chamber relatively low, for example by not applying additional heating in addition to the laser beam, a high cooling rate and lower temperature after resolidification is obtained. It is also possible to apply active cooling to remove heat from the solidified material during the laser processing to obtain an even higher cooling rate and/or lower temperature after resolidification. Active cooling can be carried out for example by means of cooling the support platform or by means of a flow of cooled gas.
- When the laser sintering process is finished, the unsintered powder is removed and the laser sintered object is removed from the build container 1. The laser sintered object is a stainless steel object having less than 20% of the austenitic phase.
- For specific applications the
object 3 is post-treated. Heat treatment can be carried out at a variety of temperatures to develop specific properties. For example, the eight standard heat treatments H900, H925, H1025, H1075, H1100, H1150, H1150+1150, H1150-M can be carried out. Also, solution annealing (SA) can be carried out to obtain desired properties. It has been observed that high cooling rates to a relatively low temperature during laser processing are essential in order to obtain a complete martensitic transformation and to avoid excess amount of remaining austenite phase in the resolidified metal. This is important for the subsequent post-treatments like H900, H925, H1025, etc. if the treatments are to be done without solution annealing and quenching. If the cooling rate is not sufficient and the martensitic transformation is only partial then additional solution annealing and subsequent quench is needed to obtain a fully martensitic phase structure which is more favourable for post-hardening treatments like H900, H925. - The method according to the invention has the additional advantage that by carrying out the laser processing with rapid cooling and resolidification, additional steps of post-treatment such as solution annealing and quenching can be omitted. Hence, the process chain becomes shorter.
-
FIG. 3 a) to 3 c) show a typical tensile testing behaviour of a laser sintered specimen. The tensile testing behaviour has been tested with a 3.56 mm thick flat test specimen according to MPIF 10 standard. -
FIG. 3 a) shows the result for a specimen produced using known stainless steel powder 17-4 PH. -
FIG. 3 b) shows a typical tensile testing behaviour of specimens produced using the metal powder according to the above described more preferred embodiment of the invention. C1, C2 and C3 are measurement results from three specimens manufactured under the same conditions, i.e. identical process parameters and geometries. -
FIG. 3 c) shows a typical tensile testing behaviour of specimens which are aged according to H900 condition after laser sintering. D1, D2 and D3 are measurement results of three specimens with the same process parameters and the same H900 heat treatment condition. As can be seen from the comparison with the prior art, the object produced using the metal powder according to the invention has considerably higher strength than the object which is produced using known stainless steel powder. Strength can be enhanced further by using heat treatment. -
FIG. 4 shows the yield and ultimate tensile strength of objects produced by laser sintering using the metal powder according to the above preferred embodiment wherein the object underwent various heat treatment conditions, respectively. As can be seen, the precipitation hardening is applicable. - In the following, the mechanical properties of an object produced using the known stainless steel 17-4 PH powder are compared to an identical object produced using the metal powder according to the invention and which was H900 heat treated after finishing the laser sintering process.
-
object produced using object produced using metal powder known stainless steel according to invention Property powder 17-4 PH H900 heat treated Ultimate tensile strength, 1050 ± 50 MPa 1486 ± 50 MPa MPa (152 ± 7 ksi) (216 ± 7 ksi) Yield strength 540 ± 50 MPa 1382 ± 50 MPa (Rp 0.2%), MPa (78 ± 7 ksi) (200 ± 7 ksi) Young's Modulus (GPa) 180 ± 20 GPa 190 ± 20 GPa (26 ± 3 msi) (28 ± 3 msi) Remaining elongation 30 ± 5% 5 ± 2% Surface hardness as laser-sintered 230 ± 20 HV1 30 ± 5 HRC H900 aged xxxxxx 43 ± 3 HRC - HV1 is the hardness in Vickers units using 1 kg load for testing; HRC is the hardness in Rockwell C scale.
- The objects produced with laser sintering and using the metal powder according to the invention, are stronger, stiffer and harder than that produced using the powder according to the prior art. Preferably, a heat treatment comprising ageing at 482° C. for one hour and air cooling provides superior mechanical properties due to precipitation hardening. Solution annealing and quenching is not required before the ageing treatment.
- All numerical values given above are to be understood as including the usual measuring tolerances.
- The metal powder according to the invention is not limited to the examples described above. For example the metal powder can be a blend of different component powders. The blend of component powders has to be selected such that the resulting powder mixture has in total a chemical composition and grain size distribution identical or similar to the powder embodiments described above. The individual component powders in the blend can differ in grain size and/or in chemistry. When they differ in chemical composition, the alloying to the final stoichiometry takes place during the laser sintering process. It is also possible that the metal powder is a blend of different component powders each having the above composition but which have different particle size distributions. Such blends can be beneficial for fine tuning the chemical composition and the grain size distribution of the resulting blended powder.
- The invention is not limited in the application to the laser sintering technique. Moreover, electron beam sintering or melting or mask sintering using a spacious heat source can also be used. The invention is not even limited to additive layer-wise production methods but includes other additive and free-form production methods of three-dimensional objects such as, for example, the 3D laser-cladding method.
Claims (41)
1. A metal powder for use in an additive production method of three-dimensional objects wherein the powder is solidified by means of a laser or electron beam or another heat source, wherein
the powder comprises iron and the following components by weight percent (wt.-%)
carbon: 0.07 max. wt-%,
chromium: 14.00-15.50 wt.-%,
nickel: 3.5-5.0 wt.-%, and
copper 3.0-4.5 wt.-%
and wherein the powder particles have a median particle size d50 between 20 μm and 100 μm.
2. The metal powder according to claim 1 , wherein the powder particles have an approximately spherical shape.
3. The metal powder according to claim 1 , wherein the powder is produced by atomisation.
4. The metal powder according to claim 1 , wherein the component elements are contained in each powder particle in a pre-alloyed manner.
5. The metal powder according to claim 1 , wherein the powder is a blend of different component powders having different grain size distributions and/or chemical compositions.
6. The metal powder according to claim 1 , further comprising 1.00 max. wt.-% of manganese.
7. The metal powder according to claim 1 , further comprising 0.03 max. wt.-% of phosphorus.
8. The metal powder according to claim 1 , further comprising 1.015 max. wt.-% of sulfur.
9. The metal powder according to claim 1 , further comprising 1.00 max. wt.-% of silicon.
10. The metal powder according to claim 1 , further comprising between 0.5 max. wt.-% molybdenum.
11. The metal powder according to claim 1 , further comprising 0.15 and 0.45 wt.-% niobium.
12. The metal powder according to claim 1 , further comprising 0.10 max. wt.-% nitrogen.
13. The metal powder according to claim 1 , wherein the content of ferrite is less than 5 wt.-%.
14. The metal powder according to claim 1 , characterized in that the powder is in the martensitic state.
15. The metal powder according to claim 1 , comprising
carbon: 0.02 (max. 0.04) wt.-%
phosphorus: 0.01 (max. 0.02) wt.-%
silicon: 0.4 (max. 0.6) wt.-%
nickel: 4.2±0.2 wt.-%
copper: 3.6±0.2 wt.-%
manganese: 0.1 (max. 0.2) wt.-%
sulfur: 0.01 (max. 0.01) wt.-%
chromium: 14.3±0.2 wt.-%
molybdenum: 0.0 (max. 0.2) wt.-%
niobium: 0.3±0.05 wt.-%
Iron: balance
Nitrogen: 0.04 (max. 0.08) wt.-%
16. A method for the production of three-dimensional objects from a powder, wherein the powder is applied in an additive manner and is solidified by means of a laser or electron beam or another heat source, wherein the powder used is a powder according to claim 1 .
17. The method according to claim 16 , wherein the powder is applied in a layer-wise manner and selectively solidified in each layer at locations corresponding to the cross-section of the object.
18. The method according to claim 16 , wherein a laser beam is used with a laser power between 20 W and 1 kW, preferably approximately 200 W.
19. The method according to claim 16 , wherein the focused laser beam spot size at the powder melting level is between 20 μm and 500 μm, preferably approximately 120 μm.
20. The method according to claim 16 , wherein the laser scanning velocity is between 50 mm/s and 10000 mm/s, preferably approximately 1000 mm/s.
21. The method according to claim 17 , wherein the distance between adjacent scan lines is between 0.02 and 0.5 mm, preferably approximately 0.1 mm.
22. The method according to claim 17 , wherein the thickness of the powder layer is between 10 μm and 200 μm, preferably approximately 20 μm.
23. The method according to claim 16 , wherein the object is precipitation hardened after the layer-wise formation.
24. The method according to claim 16 further comprises a step of cooling during the additive production method.
25. The method according to claim 16 wherein the process parameters are selected such that the object comprises less than approximately 20% of the austenitic phase.
26. A product produced by the method according to claim 16 .
27. A metal powder for use in an additive production method of three-dimensional objects wherein the powder is solidified by means of a laser or electron beam or another heat source, wherein
the powder comprises iron and the following components by weight percent (wt.-%)
carbon: 0.02 to 0.04 wt.-%
phosphorus: max. 0.02 wt.-%
silicon: 0.4 to 0.6 wt.-%
nickel: 4.2±0.2 wt.-%
copper: 3.6±0.2 wt.-%
manganese: max. 0.2 wt.-%
sulfur: max. 0.01 wt.-%
chromium: 14.3±0.2 wt.-%
molybdenum: max. 0.2 wt.-%
niobium: 0.3±0.05 wt.-%
Iron: balance
Nitrogen: max. 0.08 wt.-%
and wherein the powder particles have a median particle size d50 between 20 μm and 100 μm.
28. The metal powder according to claim 1 , wherein the powder particles have a median particle size d50 between 30 μm and 50 μm.
29. The metal powder according to claim 27 , wherein the powder particles have a median particle size d50 between 30 μm and 50 μm.
30. A method for the production of three-dimensional objects from a powder, wherein the powder is applied in an additive manner and is solidified by means of a laser or electron beam or another heat source, wherein the powder used is a powder according to claim 27 .
31. A method for the production of three-dimensional objects from a powder, wherein the powder is applied in an additive manner and is solidified by means of a laser or electron beam or another heat source, wherein the powder used is a powder according to claim 28 .
32. A method for the production of three-dimensional objects from a powder, wherein the powder is applied in an additive manner and is solidified by means of a laser or electron beam or another heat source, wherein the powder used is a powder according to claim 29 .
33. A metal powder for use in an additive production method of three-dimensional objects wherein the powder is solidified by means of a laser or electron beam or another heat source, wherein
the powder comprises iron and the following components by weight percent (wt.-%)
carbon: 0.07 max. wt-%,
chromium: 14.00-15.50 wt.-%,
nickel: 3.5-5.0 wt.-%,
copper 3.0-4.5 wt.-%,
silicon: 1.0 max wt.-%
manganese: 1.00 max. wt.-%
molybdenum: 0.5 max. wt.-%
niobium: 0.5 max wt.-%
and wherein the powder particles have a median particle size d50 between 20 μm and 100 μm.
34. The metal powder according to claim 33 , wherein the powder particles have a median particle size d50 between 30 μm and 50 μm.
35. A method for the production of three-dimensional objects from a powder, wherein the powder is applied in an additive manner and is solidified by means of a laser or electron beam or another heat source, wherein the powder used is a powder according to claim 33 .
36. A method for the production of three-dimensional objects from a powder, wherein the powder is applied in an additive manner and is solidified by means of a laser or electron beam or another heat source, wherein the powder used is a powder according to claim 34 .
37. A product produced by the method according to claim 30 .
38. A product produced by the method according to claim 31 .
39. A product produced by the method according to claim 32 .
40. A product produced by the method according to claim 35 .
41. A product produced by the method according to claim 36 .
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EP07009626.8A EP1992709B1 (en) | 2007-05-14 | 2007-05-14 | Metal powder for use in additive manufacturing method for the production of three-dimensional objects and method using such metal powder |
EP07009626.8 | 2007-05-14 |
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