EP3661680A1 - Systems and methods for nanofunctionalization of powders - Google Patents
Systems and methods for nanofunctionalization of powdersInfo
- Publication number
- EP3661680A1 EP3661680A1 EP18840807.4A EP18840807A EP3661680A1 EP 3661680 A1 EP3661680 A1 EP 3661680A1 EP 18840807 A EP18840807 A EP 18840807A EP 3661680 A1 EP3661680 A1 EP 3661680A1
- Authority
- EP
- European Patent Office
- Prior art keywords
- particles
- pressure vessel
- fluid
- agitated
- agitated pressure
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000843 powder Substances 0.000 title claims abstract description 110
- 238000000034 method Methods 0.000 title claims abstract description 60
- 239000002245 particle Substances 0.000 claims abstract description 206
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 97
- 239000012530 fluid Substances 0.000 claims abstract description 89
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 67
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 48
- 239000007787 solid Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 22
- 239000002923 metal particle Substances 0.000 claims abstract description 14
- 229910052751 metal Inorganic materials 0.000 claims description 41
- 239000002184 metal Substances 0.000 claims description 41
- 239000007788 liquid Substances 0.000 claims description 22
- 239000000919 ceramic Substances 0.000 claims description 18
- 238000004519 manufacturing process Methods 0.000 claims description 17
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 14
- GQPLMRYTRLFLPF-UHFFFAOYSA-N Nitrous Oxide Chemical compound [O-][N+]#N GQPLMRYTRLFLPF-UHFFFAOYSA-N 0.000 claims description 14
- 229910052719 titanium Inorganic materials 0.000 claims description 14
- 239000010936 titanium Substances 0.000 claims description 14
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 13
- 238000013019 agitation Methods 0.000 claims description 12
- 238000004891 communication Methods 0.000 claims description 10
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 9
- 229910052749 magnesium Inorganic materials 0.000 claims description 9
- 239000011777 magnesium Substances 0.000 claims description 9
- 150000002739 metals Chemical class 0.000 claims description 9
- 229910052725 zinc Inorganic materials 0.000 claims description 9
- 239000011701 zinc Substances 0.000 claims description 9
- 229910052726 zirconium Inorganic materials 0.000 claims description 9
- 229910052802 copper Inorganic materials 0.000 claims description 8
- 239000010949 copper Substances 0.000 claims description 8
- 150000004678 hydrides Chemical class 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 8
- 229910052744 lithium Inorganic materials 0.000 claims description 8
- 150000001247 metal acetylides Chemical class 0.000 claims description 8
- 229910052759 nickel Inorganic materials 0.000 claims description 8
- 229910052758 niobium Inorganic materials 0.000 claims description 8
- 239000010955 niobium Substances 0.000 claims description 8
- 150000004767 nitrides Chemical class 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 229910052715 tantalum Inorganic materials 0.000 claims description 8
- 229910052720 vanadium Inorganic materials 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- 229910052804 chromium Inorganic materials 0.000 claims description 7
- 239000011651 chromium Substances 0.000 claims description 7
- 229910052733 gallium Inorganic materials 0.000 claims description 7
- 229930195733 hydrocarbon Natural products 0.000 claims description 7
- 150000002430 hydrocarbons Chemical class 0.000 claims description 7
- GUCVJGMIXFAOAE-UHFFFAOYSA-N niobium atom Chemical compound [Nb] GUCVJGMIXFAOAE-UHFFFAOYSA-N 0.000 claims description 7
- 229910052709 silver Inorganic materials 0.000 claims description 7
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 claims description 7
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 6
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 6
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 6
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 6
- 229910052797 bismuth Inorganic materials 0.000 claims description 6
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 6
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 6
- 239000001272 nitrous oxide Substances 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- 239000004332 silver Substances 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000000155 melt Substances 0.000 claims description 3
- LEONUFNNVUYDNQ-UHFFFAOYSA-N vanadium atom Chemical compound [V] LEONUFNNVUYDNQ-UHFFFAOYSA-N 0.000 claims 2
- 239000002105 nanoparticle Substances 0.000 abstract description 73
- 239000011859 microparticle Substances 0.000 description 24
- 239000000463 material Substances 0.000 description 22
- 229910001092 metal group alloy Inorganic materials 0.000 description 22
- 238000000576 coating method Methods 0.000 description 21
- 239000011248 coating agent Substances 0.000 description 20
- 238000007306 functionalization reaction Methods 0.000 description 17
- 239000000654 additive Substances 0.000 description 11
- 230000000996 additive effect Effects 0.000 description 11
- 239000007789 gas Substances 0.000 description 9
- 238000012986 modification Methods 0.000 description 9
- 230000004048 modification Effects 0.000 description 9
- 238000007711 solidification Methods 0.000 description 9
- 230000008023 solidification Effects 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 8
- 229910045601 alloy Inorganic materials 0.000 description 7
- 239000000956 alloy Substances 0.000 description 7
- 230000007547 defect Effects 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 238000007670 refining Methods 0.000 description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 6
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 6
- 238000002156 mixing Methods 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- 238000005086 pumping Methods 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 6
- 239000011800 void material Substances 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 230000008901 benefit Effects 0.000 description 5
- 229910052799 carbon Inorganic materials 0.000 description 5
- 238000013461 design Methods 0.000 description 5
- 239000010410 layer Substances 0.000 description 5
- 239000012254 powdered material Substances 0.000 description 5
- 239000002243 precursor Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000006557 surface reaction Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 229910000838 Al alloy Inorganic materials 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 238000005411 Van der Waals force Methods 0.000 description 4
- 238000005275 alloying Methods 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 4
- 239000002356 single layer Substances 0.000 description 4
- GPPXJZIENCGNKB-UHFFFAOYSA-N vanadium Chemical compound [V]#[V] GPPXJZIENCGNKB-UHFFFAOYSA-N 0.000 description 4
- 125000004429 atom Chemical group 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 239000002131 composite material Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 239000011858 nanopowder Substances 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 238000012856 packing Methods 0.000 description 3
- 239000001294 propane Substances 0.000 description 3
- 239000011343 solid material Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000012546 transfer Methods 0.000 description 3
- 238000010146 3D printing Methods 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- QYEXBYZXHDUPRC-UHFFFAOYSA-N B#[Ti]#B Chemical compound B#[Ti]#B QYEXBYZXHDUPRC-UHFFFAOYSA-N 0.000 description 2
- OTMSDBZUPAUEDD-UHFFFAOYSA-N Ethane Chemical compound CC OTMSDBZUPAUEDD-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- 229910033181 TiB2 Inorganic materials 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000003623 enhancer Substances 0.000 description 2
- 238000011066 ex-situ storage Methods 0.000 description 2
- 238000009689 gas atomisation Methods 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000010348 incorporation Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 230000006911 nucleation Effects 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 230000000717 retained effect Effects 0.000 description 2
- 238000005096 rolling process Methods 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000004576 sand Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 230000001960 triggered effect Effects 0.000 description 2
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 2
- 229910000568 zirconium hydride Inorganic materials 0.000 description 2
- 235000011299 Brassica oleracea var botrytis Nutrition 0.000 description 1
- 240000003259 Brassica oleracea var. botrytis Species 0.000 description 1
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910000684 Cobalt-chrome Inorganic materials 0.000 description 1
- 229910052779 Neodymium Inorganic materials 0.000 description 1
- 241001426407 Umbrina coroides Species 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- 230000004323 axial length Effects 0.000 description 1
- 238000010923 batch production Methods 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 239000013590 bulk material Substances 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- 229910052792 caesium Inorganic materials 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 235000011089 carbon dioxide Nutrition 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- -1 cermets Substances 0.000 description 1
- 238000003889 chemical engineering Methods 0.000 description 1
- 239000010952 cobalt-chrome Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000009646 cryomilling Methods 0.000 description 1
- 210000001787 dendrite Anatomy 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000009760 electrical discharge machining Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 229910052732 germanium Inorganic materials 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910000816 inconels 718 Inorganic materials 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000001746 injection moulding Methods 0.000 description 1
- 239000001995 intermetallic alloy Substances 0.000 description 1
- 229910052741 iridium Inorganic materials 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 230000007772 nodular growth Effects 0.000 description 1
- 239000012454 non-polar solvent Substances 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 229910052762 osmium Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000010587 phase diagram Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 239000012255 powdered metal Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000003134 recirculating effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052702 rhenium Inorganic materials 0.000 description 1
- 229910052703 rhodium Inorganic materials 0.000 description 1
- 229910052701 rubidium Inorganic materials 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 238000013341 scale-up Methods 0.000 description 1
- 229910052706 scandium Inorganic materials 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000000527 sonication Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- 238000000859 sublimation Methods 0.000 description 1
- 230000008022 sublimation Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000000153 supplemental effect Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229910052713 technetium Inorganic materials 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- QSGNKXDSTRDWKA-UHFFFAOYSA-N zirconium dihydride Chemical compound [ZrH2] QSGNKXDSTRDWKA-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/02—Making metallic powder or suspensions thereof using physical processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/002—Component parts of these vessels not mentioned in B01J3/004, B01J3/006, B01J3/02 - B01J3/08; Measures taken in conjunction with the process to be carried out, e.g. safety measures
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/02—Feed or outlet devices therefor
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J3/00—Processes of utilising sub-atmospheric or super-atmospheric pressure to effect chemical or physical change of matter; Apparatus therefor
- B01J3/04—Pressure vessels, e.g. autoclaves
-
- 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
- B22F1/16—Metallic particles coated with a non-metal
-
- 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
- B22F1/18—Non-metallic particles coated with metal
-
- 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
- B22F3/003—Apparatus, e.g. furnaces
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/223—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating specially adapted for coating particles
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C24/00—Coating starting from inorganic powder
- C23C24/08—Coating starting from inorganic powder by application of heat or pressure and heat
-
- 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
-
- 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
- B22F2998/10—Processes characterised by the sequence of their steps
-
- 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
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
- B33Y70/10—Composites of different types of material, e.g. mixtures of ceramics and polymers or mixtures of metals and biomaterials
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/10—Alloys containing non-metals
-
- 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 present invention generally relates to methods and apparatus for functionalizing metal powders or other powders, and functionalized materials produced.
- Metal-based additive manufacturing, or three-dimensional (3D) printing has applications in many industries, including the aerospace and automotive industries. Building up metal components layer by layer increases design freedom and manufacturing flexibility, thereby enabling complex geometries while eliminating traditional economy-of-scale constraints.
- 3D-printable metal alloys are limited to those known to be easily weldable.
- the primary equilibrium phase solidifies first at a different composition from the bulk liquid.
- This mechanism results in solute enrichment in the liquid near the solidifying interface, locally changing the equilibrium liquidus temperature and producing an unstable, undercooled condition.
- there is a breakdown of the solid-liquid interface leading to cellular or dendritic grain growth with long channels of interdendritic liquid trapped between solidified regions.
- volumetric solidification shrinkage and thermal contraction in these channels produces cavities and hot tearing cracks which may span the entire length of the columnar grain and can propagate through additional intergranular regions.
- Fine equiaxed microstructures accommodate strain in the semi-solid state by suppressing coherency that locks the orientation of these solid dendrites and promotes tearing.
- Producing equiaxed structures requires large amounts of undercooling, which has thus far proven difficult in additive processes where high thermal gradients arise from rastering of a direct energy source in an arbitrary geometric pattern.
- Some variations of the invention provide a system for producing a functionalized powder, the system comprising:
- thermo-control unit e.g., a heater
- the fluid is a non-flammable fluid.
- the fluid may be a liquid, a gas, or a combination thereof.
- the fluid is selected from the group consisting of carbon dioxide, nitrous oxide, C 1 -C 4 hydrocarbons (e.g., methane, ethane, ethylene, propane, propylene, or n-butane), C 1 -C 4 oxygenates (e.g., methanol, ethanol, or acetone), and combinations thereof.
- C 1 -C 4 hydrocarbons e.g., methane, ethane, ethylene, propane, propylene, or n-butane
- C 1 -C 4 oxygenates e.g., methanol, ethanol, or acetone
- the fluid includes or consists essentially of carbon dioxide (C0 2 ).
- the carbon dioxide may be in a vapor state within the agitated pressure vessel. Alternatively, or additionally, the carbon dioxide may be in a liquid state within the agitated pressure vessel. In certain embodiments, the carbon dioxide is in a supercritical state within the agitated pressure vessel.
- the system optionally comprises a means for introducing solid carbon dioxide into the agitated pressure vessel.
- the exhaust line includes a filter to capture the first particles, the second particles, and/or the functionalized powder.
- the system further comprises a safety release line that is activated when the pressure within the agitated pressure vessel reaches a predetermined pressure, such as 200 bar.
- the system may further comprise a separate container disposed in flow communication with the exhaust line, for receiving fluid released from the agitated pressure vessel.
- the separate container may be a drum filled with water or oil, for example.
- the system preferably includes a control subsystem for adjusting temperature, pressure, residence time, and/or agitation within the agitated pressure vessel.
- the system may be a batch apparatus, a continuous apparatus, a semi- continuous apparatus, or a combination thereof.
- the first particles are selected from the group consisting of metal particles, intermetallic particles, ceramic particles, and
- the first particles may contain one or more metals selected from the group consisting of aluminum, iron, nickel, copper, titanium, magnesium, zinc, silicon, lithium, silver, chromium, manganese, vanadium, bismuth, gallium, lead, and combinations thereof.
- the first particles may have an average first- particle size from about 1 micron to about 1 millimeter, for example.
- the second particles are selected from the group consisting of metal particles, intermetallic particles, ceramic particles, and
- the second particles may contain one or more elements selected from the group consisting of zirconium, tantalum, niobium, titanium, and oxides, nitrides, hydrides, carbides, or borides thereof, and combinations of the foregoing.
- the second particles may have an average second-particle size from about 1 nanometer to about 100 microns, for example.
- the recovered functionalized powder is a nanofunctionalized metal powder.
- thermo-control unit e.g., a heater
- a means for introducing a plurality of second particles into the agitated pressure vessel such as by adding the second particles to a batch vessel, or pumping the second particles into continuous vessel, with or separate from the first particles;
- a means for introducing a fluid into the agitated pressure vessel such as by adding the fluid directly to the pressure vessel or by introducing a fluid precursor (e.g., solid C0 2 ) into the pressure vessel;
- a fluid precursor e.g., solid C0 2
- an exhaust line for releasing the fluid from the agitated pressure vessel, wherein the release may be continuous, intermittent, or triggered at a predetermined pressure, for example;
- a means for recovering a functionalized powder containing the second particles disposed onto surfaces of the first particles wherein the recovering may include isolating from a batch vessel, or pumping out of a continuous vessel, for example.
- Some variations of the invention provide a method for producing a functionalized powder, the method comprising:
- the fluid is selected from the group consisting of carbon dioxide, nitrous oxide, C 1 -C 4 hydrocarbons, C 1 -C 4 oxygenates, and combinations thereof.
- the fluid includes carbon dioxide in a vapor state and/or a liquid state within the agitated pressure vessel. In certain embodiments, the fluid includes carbon dioxide in a supercritical state within the agitated pressure vessel.
- solid carbon dioxide may be introduced into the agitated pressure vessel.
- the solid carbon dioxide melts within the agitated pressure vessel to form carbon dioxide in vapor form and/or liquid form.
- the C0 2 may be in vapor, liquid, and/or supercritical form, but should not be primarily in solid form.
- the reaction for reacting the second particles with the first particles is conducted at a reaction temperature from about 10°C to about 200°C. In these or other embodiments, the reaction is conducted at a reaction pressure from about 2 bar to about 200 bar. The reaction may be conducted for a reaction time from about 10 minutes to about 50 hours, for example.
- the method is operated in batch. In other embodiments, the method is operated continuously or semi-continuously.
- the first particles are selected from the group consisting of metal particles, intermetallic particles, ceramic particles, and
- the first particles contain one or more metals selected from the group consisting of aluminum, iron, nickel, copper, titanium, magnesium, zinc, silicon, lithium, silver, chromium, manganese, vanadium, bismuth, gallium, lead, and combinations thereof.
- the second particles are selected from the group consisting of metal particles, intermetallic particles, ceramic particles, and
- the second particles contain one or more elements selected from the group consisting of zirconium, tantalum, niobium, titanium, and oxides, nitrides, hydrides, carbides, or borides thereof, and combinations of the foregoing.
- FIG. 1 is an exemplary system to produce nanofunctionalized metal powder, in some embodiments of the invention.
- FIG. 2 is a flowchart for an exemplary method of using the system of
- FIG. 1 to produce a nanofunctionalized metal powder, in some embodiments.
- FIG. 3 is a scanning electron microscopy (SEM) image of Al 7075 powder nanofunctionalized with TiB 2 nanoparticles (scale bar 5 ⁇ ), in some embodiments.
- FIG. 4 is an SEM image of Al 7075 powder nanofunctionalized with
- WC tungsten carbide nanoparticles (scale bar 5 ⁇ ), in some embodiments.
- FIG. 5 is an SEM image of AlSilOMg powder nanofunctionalized with
- WC nanoparticles (scale bar 5 ⁇ ), in some embodiments.
- the present invention is premised on scalable and cost-effective systems for powder functionalization without requiring flammable solvents.
- the functionalized powders may be used in additive manufacturing or as raw materials in other applications that can benefit from powder functionalization.
- Some variations of the invention provide a system for producing a functionalized powder, the system comprising:
- thermo-control unit such as a heater
- the choice of fluid(s) will depend on compatibility of fluid with the first and second particles.
- the fluid dissolves or suspends at least one of the components. Van der Waals forces, chemical bonds, physical adsorption, or other forces may cause the second particles to be retained on surfaces of the first particles.
- the fluid may have a lower surface energy than the first particles, the second particles, or both of these. When this fluid is released from a mixture of first and second particles, the latter may be drawn by capillary forces to surfaces of first particles, in some embodiments.
- the fluid may be a liquid, a gas, or a combination thereof.
- the fluid is selected from the group consisting of carbon dioxide (C0 2 ) nitrous oxide (N 2 0), C 1 -C 4 hydrocarbons (e.g., methane, ethane, ethylene, propane, propylene, or n-butane), C 1 -C 4 oxygenates (e.g., methanol, ethanol, or acetone), and combinations thereof.
- C 1 -C 4 hydrocarbons e.g., methane, ethane, ethylene, propane, propylene, or n-butane
- C 1 -C 4 oxygenates e.g., methanol, ethanol, or acetone
- derivatives of hydrocarbons or oxygenates in which one or more hydrogen atoms are replaced by other elements or functional groups, are included.
- replacing each H atom with a CI atom in methane results in carbon tetrachloride (CC1 4 ),
- the fluid is a non-flammable fluid.
- a "nonflammable fluid” as meant herein is a fluid that does not combust in air at atmospheric pressure. Exemplary non-flammable fluids are C0 2 , N 2 0, and CC1 4 .
- an ordinarily flammable substance such as propane
- the fluid includes or consists essentially of carbon dioxide.
- the carbon dioxide may be in a vapor state within the agitated pressure vessel. Alternatively, or additionally, the carbon dioxide may be in a liquid state within the agitated pressure vessel. In certain embodiments, the carbon dioxide is in a supercritical state within the agitated pressure vessel.
- the system optionally comprises a means for introducing solid carbon dioxide (also known as dry ice) into the agitated pressure vessel.
- the C0 2 may be vented off quickly and recycled, thereby eliminating waste while also drying the powder. Following removal of liquefied or supercritical C0 2 , Van der Waals forces, chemical bonds, physical adsorption, or other forces may cause the nanoparticles to be retained on surfaces of the powder particles.
- the agitated pressure vessel is operated under effective reaction conditions to dispose the second particles onto surfaces of the first particles, regardless of mechanism.
- the effective reaction conditions include selection of temperature, pressure, residence time (i.e., reaction time), and agitation, or ranges of such parameters, such that the desired powder functionalization takes place at least to some extent.
- Effective temperatures may range from about 10°C to about 200°C, such as from about 25°C to about 100°C, e.g. about 30°C, 35°C, 40°C, 50°C, 60°C, 70°C, 80°C, or 90°C.
- the thermal-control unit may be omitted.
- the thermal-control unit may be a heater, which may be provided in various forms such as (but not limited to) hot oil, steam jacket, heat tape, or an oven, for example.
- the thermal-control unit may be a combined heater/cooler or a heat-transfer medium that enables the reactor to be maintained at a desired temperature.
- Effective pressures may range from about 2 bar to about 200 bar, such as from about 10, 20, 30, 40, 50, 60, 70, 80, 90, or 100 bar.
- Effective residence times may range from about 1 minute to about 100 hours, such as from about 10 minutes to about 50 hours, e.g. about 0.5, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 15, 20, or 25 hours.
- Selection of temperature and pressure will generally depend on choice of fluid, and one skilled in the art can consult the phase diagram of the selected fluid so that the fluid, during particle functionalization, remains in the desired phase(s) such as a liquid phase or the supercritical phase.
- Selection of time will generally depend on the nature of the first and second particles and the kinetics associated with functionalization, which depends on selected temperature and pressure. There is therefore an interrelationship among time, temperature, and pressure, as is common with chemical reactions.
- the pressure vessel may be agitated in a variety of ways.
- the pressure vessel is disposed in physical communication with an external vibrating motor that physically vibrates the pressure vessel to mix the contents.
- the pressure vessel is configured with a stirring mechanism such as an internal impeller or paddle.
- the pressure vessel is agitated by rolling or tumbling the pressure vessel in an automated manner within the overall system.
- the pressure vessel is agitated via continuous recycling of fluid that is pumped out of and back into the pressure vessel. For example, a continuous purge of fluid may be taken from the pressure vessel, separate from or integrated with the exhaust line, from the top and reinjected into the bottom of the pressure vessel to enhance the mixing efficiency.
- continuous recirculation of an inert gas (such as Ar or N 2 ) through the pressure vessel may be employed to enhance the mixing efficiency.
- an inert gas such as Ar or N 2
- Combinations of any of these agitation techniques, or others may be employed in certain embodiments.
- Effective agitation ranges may vary and may be characterized by an output associated with the selected agitation means.
- the vibration frequency may be monitored or controlled.
- the impeller revolution frequency e.g., revolutions per minute, rpm
- the recycle flow rate may be monitored or controlled, and so on.
- the fluid Reynolds Number (Re) may be monitored, estimated, or controlled, such as by use of tracers to measure velocity distribution within the pressure vessel.
- the Re may be based on the vessel diameter or on the impeller diameter in the case of an internal impeller, for example.
- an effective internal Re may be from about 100 to about 10,000, such as from about 1,000 to about 5,000.
- the flow pattern within the pressure vessel may be laminar or turbulent.
- the system preferably includes a reactor control subsystem for adjusting temperature, pressure, residence time, and/or agitation within the agitated pressure vessel.
- a reactor control subsystem may be configured to vary parameters during reaction, such as over a prescribed protocol, or in response to measured variables. For example, an unintended change in vessel pressure may be compensated by a change in vessel temperature and/or residence time. As another example, temperature may be maintained constant (isothermal operation) or pressure may be maintained constant (isobaric operation).
- the reactor control subsystem may utilize well-known control logic principles, such as feedback control and feedforward control. Control logic may incorporate results from previous experiments or production campaigns.
- One example of a reactor control subsystem is MasterLogic Programmable Logic Controller from Honeywell (Morris Plains, New Jersey, U.S.).
- the pressure within the pressure vessel may be reduced or fully released (i.e. down to atmospheric pressure) by opening a valve to allow the fluid to exit out the exhaust line.
- the pressure vessel may be opened and the functionalized powder may be allowed to dry before recovery from the vessel.
- an inert gas is swept through the vessel following such pressure release, to assist in drying by removing residual fluid, for example.
- the pressure vessel may be reduced or fully released (i.e. down to atmospheric pressure) by opening a valve to allow the fluid to exit out the exhaust line.
- the pressure vessel may be opened and the functionalized powder may be allowed to dry before recovery from the vessel.
- an inert gas is swept through the vessel following such pressure release, to assist in drying by removing residual fluid, for example.
- the pressure within the pressure vessel may be reduced or fully released (i.e. down to atmospheric pressure) by opening a valve to allow the fluid to exit out the exhaust line.
- the pressure vessel may be opened and the functionalized powder may be allowed to dry before recovery from the vessel.
- the functionalized powder may be recovered from the pressure vessel and introduced into a separate unit for drying or other treatment.
- the pressure vessel may be configured with a large valve and optionally a bottom scraper or other means to recover the functionalized powder from the pressure vessel.
- the system may further comprise a separate container disposed in flow communication with the exhaust line, for receiving fluid released from the agitated pressure vessel.
- the separate container may be a drum filled with water or oil, for example.
- Particles or functionalized powder preferably should not be allowed to flow to the separate container.
- particles and functionalized powder may end up in the exhaust line.
- the exhaust line includes a filter to capture the first particles, the second particles, and/or the functionalized powder.
- the filter may be designed to remove particles that are at least the size of nanoparticles, at least the size of microparticles, or some other filter size.
- a centrifuge or other separation means is utilized in the exhaust line, to recover the filtered solid material.
- the recovered solid material (e.g., from filtering, centrifuging, or other means) may then be returned to the pressure vessel, either continuously or intermittently, or discarded.
- the system further comprises a safety release line that is activated when the pressure within the agitated pressure vessel reaches or exceeds a predetermined pressure, such as a pressure selected from 25 bar to 300 bar (e.g., 200 bar) that is higher than the desired reaction pressure within the pressure vessel.
- a predetermined pressure such as a pressure selected from 25 bar to 300 bar (e.g., 200 bar) that is higher than the desired reaction pressure within the pressure vessel.
- the reactor control subsystem mentioned above may include protective devices that automatically shut down the operation, when the temperature or pressure exceeds a maximum value.
- Practical safety-related design may be built into the system as well. For example, the entire pressure vessel may be disposed within a sand bath contained in a suitable container. Those skilled in the art will understand how to design safe pressure vessels and systems employing them.
- the volume of the pressure vessel may vary widely, such as (but not limited to) from about 0.1 liter to about 1,000 liters, e.g. from about 1 liter to about 100 liters.
- the system may be a batch apparatus, a continuous apparatus, a semi- continuous apparatus, or a combination thereof.
- a batch apparatus includes a batch reactor, such as a pressure vessel. An example of a pressure vessel as a batch reactor is depicted in FIG. 1, further discussed below.
- a continuous apparatus includes a high-pressure reactor configured for a continuous feed of first and second particles and a continuous feed of fluid.
- the high-pressure reactor may be a tank or vessel in which the particles and fluid are continuously stirred, or a tubular reactor in which the particles and fluid are in plug flow (which is well-mixed, i.e. agitated, in the radial direction), or an intermediate mixing pattern between these extremes.
- a continuous high-pressure reactor may be horizontal or vertical, and may be configured for cocurrent flow of particles and fluid, or countercurrent flow of particles and fluid, or countercurrent flow of fluid and first particles against flow of second particles, and so on.
- An example of a semi-continuous apparatus is the batch apparatus of FIG. 1 modified for continuous recirculating flow of fluid, or a continuously stirred tank with intermittent feed of particles and/or intermittent release of fluid, for example.
- the first particles are selected from the group consisting of metal particles, intermetallic particles, ceramic particles, and
- the first particles may contain one or more metals selected from the group consisting of aluminum, iron, nickel, copper, titanium, magnesium, zinc, silicon, lithium, silver, chromium, manganese, vanadium, bismuth, gallium, lead, and combinations thereof.
- the first particles may have an average first-particle size from about 1 micron to about 1 millimeter, for example. In various embodiments, the first particles have an average first-particle size of about 1, 2, 5, 10, 25, 50, 100, 200, 300, 400, 500, 600, 700, 800, or 900 microns.
- the second particles are selected from the group consisting of metal particles, intermetallic particles, ceramic particles, and combinations thereof.
- the second particles may contain one or more elements selected from the group consisting of zirconium, tantalum, niobium, titanium, and oxides, nitrides, hydrides, carbides, or borides thereof, and combinations of the foregoing.
- the second particles may have an average second-particle size from about 1 nanometer to about 100 microns, for example.
- the second particles have an average second-particle size of about 1, 2, 5, 10, 25, 50, 100, 200, 300, 400, 500, 600, 700, 800, or 900 nanometers, or about 1, 2, 5, 10, 20, 30, 40, 50, or 75 microns.
- the recovered functionalized powder is a nanofunctionalized metal powder.
- the average second-particle size is 1000 nanometers or less.
- thermo-control unit disposed in thermal communication with the agitated pressure vessel
- a means for introducing a plurality of second particles into the agitated pressure vessel such as by adding the second particles to a batch vessel, or pumping the second particles into continuous vessel, with or separate from the first particles;
- a means for introducing a fluid into the agitated pressure vessel such as by adding the fluid directly to the pressure vessel or by introducing a fluid precursor (e.g., inserting solid C0 2 prior to starting the reaction) into the pressure vessel;
- an exhaust line for releasing the fluid from the agitated pressure vessel, wherein the release may be continuous, intermittent, or triggered at a predetermined pressure, for example;
- a means for recovering a functionalized powder containing the second particles disposed onto surfaces of the first particles wherein the means for recovering may include isolating from a batch vessel, or pumping out of a continuous vessel, for example.
- FIG. 1 is an exemplary system for producing a functionalized powder. This design can be adapted using known chemical-engineering principles to any scale system for continued production of larger volumes of functionalized powders.
- the example system of FIG. 1 is capable of containing a controlled volume of carbon dioxide above its critical point, and is capable of safely immersing metal powders in a supercritical carbon dioxide environment.
- FIG. 1 is a process-flow diagram of a particle functionalization system
- a pressure vessel 105 may be a metal vessel manufactured by Parr Instrument Company (Moline, Illinois, US) with an interior volume of 1 liter.
- the pressure vessel 105 is disposed within an outer container 160, in some embodiments.
- System 100 is a closed environment to avoid the unintended escape of particles from the system.
- the pressure vessel 105 contains metal powders as the first particles, and metal or non-metal nanopowders as the second particles.
- the selected fluid is carbon dioxide, in this example.
- the carbon dioxide, metal powder, and nanopowder may be enclosed in the pressure vessel 105 in a batchwise manner, i.e. prior to closing up the pressure vessel 105 for operation.
- the carbon dioxide may be sealed in the pressure vessel 105 in its solid state, along with packing the particles into the pressure vessel 105.
- the packing may be done in an inert atmosphere, such as with argon or nitrogen.
- the solid carbon dioxide undergoes sublimation to form C0 2 gas, prior to operation of the pressure vessel. Depending on the time to begin operation, some of the solid C0 2 may melt into liquid C0 2 or convert to supercritical C0 2 without first sublimating into vapor. Regardless of the form of C0 2 added to the pressure vessel 105, the temperature and pressure during functionalization will dictate the phase(s) of C0 2 present in the pressure vessel 105.
- the pressure vessel 105 is attached to a heating element 110.
- the heating element 110 e.g., heat tape
- the pressure vessel 105 may be insulated to maintain adiabatic operation or at least minimize heat losses. External cooling of the pressure vessel 105 may be employed in certain embodiments in which functionalization is exothermic, to help control reaction temperature.
- a vibrating motor 115 is directly attached to the surface of the vessel
- the vessel 105 may be agitated by other known agitation means such as stirring, rolling, tumbling, etc.
- the pressure vessel 105 of FIG. 1 includes a general inlet/outlet at the top of the vessel.
- the general inlet/outlet is directly attached to a pressure transducer 125, which has an electrical readout of 0-5 VDC to be calibrated and used in
- the pressure transducer 125 is in line with a pneumatically controlled valve 135, which will open such as when 5-15 bar air pressure is applied to its actuator.
- the actuator may be controlled remotely by an air compressor 130.
- a partially opened needle valve 140 restricts the flow rate of fluid out of the system.
- a flexible stainless steel braided hose may make this connection.
- the pneumatically controlled valve 135 keeps the vessel release line
- valve 135 closed during standard operation.
- the valve 135 may be opened remotely by applying a change in pressure.
- the flow of the fluid and particles through the release line 145 may be limited by the needle valve 140.
- the released fluid, C0 2 in this example may be fed via release line 145 into a drum of water or another container (not shown).
- An overpressure line 155 may be routed to the same drum of water or other container, or otherwise purged from the system.
- the over-pressure line 155 is primarily for safety and is not normally in operation.
- an over-pressure rupture disk or an automated pressure-relief valve is disposed in flow communication with an orifice of the pressure vessel.
- the over-pressure rupture disk or automated pressure-relief valve may be connected to a line that leads to the same container (e.g., 55-gallon drum of water) that receives the fluid release line.
- the over-pressure rupture disk or automated pressure-relief valve may be configured to burst or release at any desired pressure, such as a pressure selected from 100-300 bar (e.g., 200 bar).
- the entire vessel 105 may be submerged in a 55-gallon drum filled with sand, as the outer container 160, for example.
- a sand drum 160 is also for safety and may be omitted when the pressure vessel 105 is properly prevented from explosion.
- Some variations of the invention provide a method for producing a functionalized powder, the method comprising:
- the fluid is selected from the group consisting of carbon dioxide, nitrous oxide, C 1 -C 4 hydrocarbons, C 1 -C 4 oxygenates, and combinations thereof.
- the fluid includes carbon dioxide in a vapor state and/or a liquid state within the agitated pressure vessel. In certain embodiments, the fluid includes carbon dioxide in a supercritical state within the agitated pressure vessel.
- solid carbon dioxide may be introduced into the agitated pressure vessel.
- the solid carbon dioxide melts within the agitated pressure vessel to form carbon dioxide in vapor form and/or liquid form.
- the C0 2 may be in vapor, liquid, and/or supercritical form, but should not be primarily in solid form.
- the reaction for reacting the second particles with the first particles is conducted at a reaction temperature from about 10°C to about 200°C. In these or other embodiments, the reaction is conducted at a reaction pressure from about 2 bar to about 200 bar. The reaction may be conducted for a reaction time from about 10 minutes to about 50 hours, for example.
- the method is operated in batch. In other embodiments, the method is operated continuously or semi-continuously.
- the first particles are selected from the group consisting of metal particles, intermetallic particles, ceramic particles, and
- the first particles contain one or more metals selected from the group consisting of aluminum, iron, nickel, copper, titanium, magnesium, zinc, silicon, lithium, silver, chromium, manganese, vanadium, bismuth, gallium, lead, and combinations thereof.
- the second particles are selected from the group consisting of metal particles, intermetallic particles, ceramic particles, and
- the second particles contain one or more elements selected from the group consisting of zirconium, tantalum, niobium, titanium, and oxides, nitrides, hydrides, carbides, or borides thereof, and combinations of the foregoing.
- FIG. 2 is a flowchart for an exemplary method of using the system of
- FIG. 1 to produce a functionalized powder, in some embodiments.
- the system of FIG. 1 may be operated according to the method of FIG. 2.
- the system of FIG. 1 and the method of FIG. 2 are suitable for producing the exemplary functionalized metal powders shown in FIGS. 3, 4, and/or 5.
- FIG. 3 is a scanning electron microscopy (SEM) image of Al 7075 powder 310 nanofunctionalized with discontinuous TiB 2 nanoparticles 320 (scale bar 5 ⁇ ), resulting in functionalized powder 300.
- FIG. 4 is an SEM image of Al 7075 powder 410 nanofunctionalized with discontinuous WC (tungsten carbide) nanoparticles 420 (scale bar 5 ⁇ ), resulting in functionalized powder 400.
- FIG. 5 is an SEM image of AlSilOMg powder 510 nanofunctionalized with discontinuous WC nanoparticles 520 (scale bar 5 ⁇ ), resulting in functionalized powder 500.
- Functionalized feedstocks may be powder feedstocks.
- powder feedstocks refers to any powdered metal, ceramic, polymer, glass, composite, or combination thereof.
- the powder feedstocks are metals or metal-containing compounds, such as (but not limited to) Al, Mg, Ni, Fe, Cu, Ti, V, Si, or combinations thereof, for example.
- Nanoparticles or microparticles are typically a different composition than the base powder.
- Nanoparticles or microparticles may include metals, ceramics, cermets, intermetallic alloys, oxides, carbides, nitrides, borides, polymers, carbon, and combinations thereof, for example, or other materials which upon processing form one or more of the aforementioned materials.
- the functionalized materials may contain one or more alloying elements selected from the group consisting of Si, Fe, Cu, Ni, Mn, Mg, Cr, Zn, V, Ti, Bi, Ga, Pb, or Zr.
- Other alloying elements may be included, such as (but not limited to) H, Li, Be, B, C, N, O, F, Na, P, S, CI, K, Ca, Sc, Co, Zn, Ga, Ge, As, Se, Br, Rb, Sr, Y, Nb, Mo, Tc, Ru, Rh, Pd, Ag, Cd, In, Sn, Te, I, Cs, Ba, Hf, Ta, W, Re, Os, Ir, Pt, Au, Hg, TI, Ce, Nd, and combinations thereof.
- the nanoparticles or microparticles contain one or more elements selected from the group consisting of zirconium, tantalum, niobium, titanium, and combinations, oxides, nitrides, hydrides, carbides, or borides thereof.
- An exemplary zirconium hydride is ZrH 2 .
- Powder particle sizes are typically between about 1 micron and about 1 millimeter, but in some cases could be as much as about 1 centimeter.
- the powdered feedstock may be in any form in which discrete particles can be reasonably distinguished from the bulk.
- the powder may be present as loose powders, a paste, a suspension, or a green body, for example.
- a green body is an object whose main constituent is weakly bound powder material, before it has been melted and solidified.
- the functionalized powder feedstocks may be converted into a geometric object, such as a wire, by controlling melting and solidification.
- the geometric object may itself be a functionalized precursor feedstock for another process, or may be a final part.
- Powder particles may be solid, hollow, or a combination thereof.
- Particles can be made by any means including, for example, gas atomization, milling, cryomilling, wire explosion, laser ablation, electrical-discharge machining, or other techniques known in the art.
- the powder particles may be characterized by an average aspect ratio from about 1 : 1 to about 100: 1.
- the "aspect ratio” means the ratio of particle length to width, expressed as length:width.
- a perfect sphere has an aspect ratio of 1 : 1.
- the length is taken to be the maximum effective diameter and the width is taken to be the minimum effective diameter.
- particles within a powder feedstock are rod- shaped particles or domains resembling long sticks, dowels, or needles.
- the average diameter of the rod-shaped particles or domains may be selected from about 5 nanometers to about 100 microns, for example.
- Rods need not be perfect cylinders, i.e. the axis is not necessarily straight and the diameter is not necessarily a perfect circle.
- the aspect ratio is the actual axial length, along its line of curvature, divided by the effective diameter, which is the diameter of a circle having the same area as the average cross-sectional area of the actual shape.
- “Surface functionalization” refers to a surface modification on the powdered materials, which modification affects the solidification behavior (e.g., solidification rate, yield, grain quality, heat release, etc.) of the powder materials.
- a powdered material is functionalized with about 1%, 2%, 5%, 10%, 15%, 20%, 25%, 30%, 40%, 50%, 60%, 70%, 80%, 85%, 90%, 95%, 99%, or 100%) of the surface area of the powdered material having surface-functionalization modifications.
- the surface modification maybe a surface-chemistry modification, a physical surface modification, or a combination thereof.
- the surface functionalization includes a nanoparticle coating and/or a microparticle coating.
- the nanoparticles and/or microparticles may include a metal, ceramic, polymer, or carbon, or a composite or combination thereof.
- the surface functionalization preferably includes nanoparticles that are chemically or physically disposed on the surface of the powder materials.
- Nanoparticles are particles with the largest dimension between about 1 nm and about 5000 nm.
- a preferred size of nanoparticles is about 2000 nm or less, about 1500 nm or less, or about 1000 nm or less. In some embodiments,
- nanoparticles are at least 50 nm in size.
- Microparticles are particles with the largest dimension between about 1 micron and about 1000 microns.
- the ratio of average particle size of microparticles to average particle size of nanoparticles may vary, such as about 1, about 10, about 10 2 , about 10 3 , about 10 4 , or about 10 5 . In some embodiments, this ratio is from about 10 to about 1000.
- nanoparticle or microparticle size may be selected based on the desired final properties. Generally speaking, nanoparticles are preferred over microparticles for functionalization. However, references in this specification to nanoparticles should be understood to include embodiments in which microparticles are used in place of, or in addition to, nanoparticles.
- Nanoparticles or microparticles may be spherical or of arbitrary shape with the largest dimension typically not exceeding the above largest dimensions.
- An exception is structures with extremely high aspect ratios, such as carbon nanotubes in which the dimensions may include up to 100 microns in length but less than 100 nm in diameter.
- the nanoparticles or microparticles may include a coating of one or more layers of a different material. Mixtures of nanoparticles and microparticles may be used. In some embodiments, microparticles themselves are coated with
- microparticle/nanoparticle composite is incorporated as a coating or layer on the powder material particles.
- Nanoparticles or microparticles may be attached using electrostatic forces, Van der Waals forces, chemical bonds, physical bonds, and/or any other force.
- a chemical bond is the force that holds atoms together in a molecule or compound. Electrostatic and Van der Waals forces are examples of physical forces that can cause bonding.
- a physical bond is a bond that arises when molecular entities become entangled in space. Typically, chemical bonds are stronger than physical bonds. Chemical bonds may include ionic bonds, covalent bonds, or a combination thereof.
- the nanoparticles may be generated ex situ, generated in situ, or a combination thereof.
- Ex situ generation of nanoparticles means that the nanoparticles are introduced to the powder surface already in the form of nanoparticles, from a prior step.
- In situ generation of nanoparticles means that nanoparticles are made from a precursor that has already been applied, or is continuously applied, to the powder surface, within the agitated pressure vessel.
- nanoparticles may be generated in situ by pulse-wire discharge (wire explosion), solidification from a vapor phase containing nanoparticle precursors, vaporization followed by solidification, or other means.
- Assembly aids may be incorporated. Assembly aids enhance the retention of nanoparticles on surfaces of the powder particles. In particular, assembly aids may enhance the chemical kinetics of nanoparticle assembly, the
- thermodynamics of nanoparticle assembly or the diffusion or mass transport of nanoparticle assembly, for example.
- Assembly aids may be selected from the group consisting of surfactants, salts, dissolved ions, charged molecules, polar or non-polar solvents, hierarchically sized particulates, surface etchants for surface texture, and combinations thereof.
- surfactants may reduce surface tension between nanoparticles and powder surfaces, resulting in better wetting and assembly.
- Salts or ions may alter the surface charge of the nanoparticles or powder surfaces, resulting in ionic bonds that enhance the assembly.
- Surface etchants may physically etch the surface of the powder to promote adsorption of nanoparticles.
- the nanoparticles may be in the form of a monolayer, a multilayer, or less than one monolayer (e.g., from about 1% to 100% of one monolayer) and may be uniform or non-uniform at the powder surfaces.
- the exemplary materials shown in FIGS. 3 to 5 suggest non-uniform particles (discontinuous coating), forming less than one monolayer on average.
- Nanoparticles may act as grain refiners to give a unique microstructure for a component ultimately produced from a nanofunctionalized metal powder as provided herein.
- the second particles include grain-refining nanoparticles.
- the grain-refining nanoparticles may be present in a concentration of at least 0.01 vol%, such as at least 0.1 vol%, at least 1 vol%, or at least 5 vol%.
- the grain-refining nanoparticles are present in a concentration of about, or at least about, 0.1, 0.2, 0.5, 1, 2, 3, 4, 5, 6, 7, 8, 9, or 10 vol%.
- the concentration of the grain refiner(s) may be varied by adjusting the amount of grain refiners functionalized on the powder surface, and/or by adjusting the concentration of functionalized micropowders versus non-functionalized
- micropowders in the final material Routine experimentation can be performed by a person of ordinary skill in the art to inform material selection and concentration for the grain-refining nanoparticles.
- the number of nanoparticles per microparticle can vary widely.
- nanoparticles may be about 10, about 10 2 , about 10 3 , about 10 4 , about 10 5 , or about 10 6 , for example.
- the nanoparticle distribution on the powder particle surface can vary, as shown in FIGS. 3 to 5.
- surface regions contain a relatively higher concentration of nanoparticles, which may be agglomerated at the surface in those regions.
- the nanoparticle surface coverage may also vary widely, from about
- the nanoparticle surface coverage is the average area fraction of powder particles that is covered by assembled nanoparticles.
- the nanoparticle surface coverage may be about, or at least about, 1%, 5%, 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80%, 90%, or 100%. Due to the small size of nanoparticles, benefits are possible with less than 1%> surface area coverage.
- At least one nanoparticle is lattice-matched to within ⁇ 5%) compared to powder feedstock without the nanoparticle.
- the nanoparticle is lattice-matched to within ⁇ 2%, more preferably to within ⁇ 0.5%, compared to a powder feedstock without the nanoparticle.
- surface functionalization is in the form of a continuous coating or an intermittent coating.
- a continuous coating covers at least 90%) of the surface, such as about 95%, 99%, or 100% of the surface (recognizing there may be defects, voids, or impurities at the surface).
- An intermittent coating is non-continuous and covers less than 90%, such as about 80%, 70%, 60%, 50%, 40%, 30%), 20%), 10%), 5%), 2%), 1%), or less of the surface.
- An intermittent coating may be uniform (e.g., having a certain repeating pattern on the surface) or non-uniform (e.g., random).
- a functionalization coating may be continuous or discontinuous.
- the coating may have several characteristic features.
- the coating may be smooth and conformal to the underlying surface.
- the coating may be nodular.
- the nodular growth is often characteristic of kinetic limitations of nanoparticle assembly.
- the coating may look like cauliflower or a small fractal growing from the surface.
- microparticles (rather than nanoparticles) coat micropowders or macropowders.
- the micropowder or macropowder particles may include ceramic, metal, polymer, glass, or combinations thereof.
- coating may include metal, ceramic, polymer, carbon, or combinations thereof.
- functionalization preferably means that the coating particles are of significantly different dimension(s) than the base powder.
- the microparticles may be characterized by an average dimension (e.g., diameter) that is less than 20%, 10%, 5%), 2%), or 1%) of the largest dimension of the coated powders.
- the materials and methods disclosed herein may be applied to additive manufacturing as well as joining techniques, such as welding.
- Certain unweldable metals such as high-strength aluminum alloys (e.g., aluminum alloys Al 7075, Al 7050, or Al 2199) would be excellent candidates for additive manufacturing but normally suffer from hot cracking.
- the principles disclosed herein allow these alloys to be processed with significantly reduced cracking tendency.
- the nanofunctionalized metal powder may be converted to a metal alloy object through various means, such as additive manufacturing or other metal processing, wherein the metal alloy object is characterized by a unique microstructure.
- a unique microstructure may be produced in a wide variety of alloy systems, as well as from metal processing beyond additive manufacturing.
- a metal alloy microstructure (produced starting with a functionalized metal powder) is "substantially crack-free" which means that at least 99.9 vol% of the metal alloy contains no linear or tortuous cracks that are greater than 0.1 microns in width and greater than 10 microns in length.
- a defect must be a void space that is at least 0.1 microns in width as well as at least 10 microns in length.
- a void space that has a length shorter than 10 microns but larger than 1 micron, regardless of width, can be considered a porous void (see below).
- a void space that has a length of at least 10 microns but a width shorter than 0.1 microns is a molecular-level gap that is not considered a defect.
- a crack typically contains open space, which may be vacuum or may contain a gas such as air, C0 2 , N 2 , and/or Ar.
- a crack may also contain solid material different from the primary material phase of the metal alloy. These sorts of cracks containing material (other than gases) may be referred to as "inclusions.”
- the non- desirable material disposed within the inclusion may itself contain a higher porosity than the bulk material, may contain a different crystalline (or amorphous) phase of solid, or may be a different material altogether, arising from impurities during fabrication, for example. Large phase boundaries can also form inclusions. Note that these inclusions are different than the desirable nanoparticle inclusions that may form during additive manufacturing.
- the metal alloy microstructure may be substantially free of porous defects, in addition to being substantially crack-free. "Substantially free of porous defects” means at least 99 vol% of the metal alloy contains no porous voids having an effective diameter of at least 1 micron.
- Porous defects may be in the form of porous voids.
- a porous void contains open space, which may be vacuum or may contain a gas such as air, C0 2 , N 2 , and/or Ar.
- at least 80 vol%, more preferably at least 90 vol%, even more preferably at least 95 vol%, and most preferably at least 99 vol% of the metal alloy contains no porous voids having an effective diameter of at least 1 micron.
- a porous void that has an effective diameter less than 1 micron is not typically considered a defect, as it is generally difficult to detect by conventional nondestructive evaluation.
- At least 90 vol%, more preferably at least 95 vol%, even more preferably at least 99 vol%, and most preferably at least 99.9 vol% of the metal alloy contains no larger porous voids having an effective diameter of at least 5 microns.
- the metal alloy microstructure (produced starting with a functionalized metal powder) has "equiaxed grains" which means that at least 99 vol% of the metal alloy contains grains that are roughly equal in length, width, and height.
- crystals of metal alloy form grains in the solid. Each grain is a distinct crystal with its own orientation. The areas between grains are known as grain boundaries. Within each grain, the individual atoms form a crystalline lattice. Equiaxed grains result when there are many nucleation sites arising from grain-refining nanoparticles contained in the metal alloy microstructure.
- a solid metal alloy object comprising at least one solid phase (i) containing a functionalized powdered material as described, or (ii) derived from a liquid form of a functionalized powdered material as described.
- the solid metal alloy object may be a geometric object (e.g., wire or rod) that is useful for metal processing, instead of powder feedstock.
- the solid metal alloy object may be subjected to powder metallurgy processing techniques including, but are not limited to, hot pressing, low-pressure sintering, extrusion, metal injection molding, and additive manufacturing.
Abstract
Description
Claims
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
US201762540616P | 2017-08-03 | 2017-08-03 | |
US15/996,439 US11779894B2 (en) | 2017-02-01 | 2018-06-02 | Systems and methods for nanofunctionalization of powders |
PCT/US2018/035766 WO2019027563A1 (en) | 2017-08-03 | 2018-06-03 | Systems and methods for nanofunctionalization of powders |
Publications (2)
Publication Number | Publication Date |
---|---|
EP3661680A1 true EP3661680A1 (en) | 2020-06-10 |
EP3661680A4 EP3661680A4 (en) | 2021-01-06 |
Family
ID=65232964
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP18840807.4A Pending EP3661680A4 (en) | 2017-08-03 | 2018-06-03 | Systems and methods for nanofunctionalization of powders |
Country Status (3)
Country | Link |
---|---|
EP (1) | EP3661680A4 (en) |
CN (1) | CN110997197A (en) |
WO (1) | WO2019027563A1 (en) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US11154929B2 (en) | 2017-12-26 | 2021-10-26 | Daido Steel Co., Ltd. | Metal powder material |
CN115845779A (en) * | 2023-02-06 | 2023-03-28 | 河北新欣园能源股份有限公司 | Multi-functional reation kettle for chemical production |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20210146439A1 (en) * | 2019-11-18 | 2021-05-20 | Hrl Laboratories, Llc | Functionalized aspherical powder feedstocks and methods of making the same |
CN113000842B (en) * | 2021-03-08 | 2023-04-07 | 昆明理工大学 | Method for preparing alloy semi-solid thixotropic blank by continuously extruding simple substance mixed powder |
Family Cites Families (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR950703413A (en) * | 1992-11-02 | 1995-09-20 | 레오나드 디. 영 | METHOD OF PREPARING COATING MATERRIALS |
US5725987A (en) * | 1996-11-01 | 1998-03-10 | Xerox Corporation | Supercritical processes |
US6184270B1 (en) * | 1998-09-21 | 2001-02-06 | Eric J. Beckman | Production of power formulations |
US7537803B2 (en) * | 2003-04-08 | 2009-05-26 | New Jersey Institute Of Technology | Polymer coating/encapsulation of nanoparticles using a supercritical antisolvent process |
WO2005060668A2 (en) * | 2003-12-18 | 2005-07-07 | The Trustees Of Columbia University In The City Ofnew York | Methods of modifying surfaces |
US7141207B2 (en) * | 2004-08-30 | 2006-11-28 | General Motors Corporation | Aluminum/magnesium 3D-Printing rapid prototyping |
FR2900845B1 (en) * | 2006-05-15 | 2009-03-06 | Commissariat Energie Atomique | PROCESS AND DEVICE FOR SYNTHESIS OF ORGANIC OR INORGANIC COATED PARTICLES |
FR2915753B1 (en) * | 2007-05-02 | 2009-09-04 | Commissariat Energie Atomique | METHOD AND DEVICE FOR PREPARING A MULTILAYER COATING ON A SUBSTRATE |
WO2011059074A1 (en) * | 2009-11-13 | 2011-05-19 | 森六ケミカルズ株式会社 | Fine powder manufacturing method and fine powder manufactured using same |
US20130209308A1 (en) * | 2012-02-15 | 2013-08-15 | Baker Hughes Incorporated | Method of making a metallic powder and powder compact and powder and powder compact made thereby |
GB201316430D0 (en) * | 2013-09-16 | 2013-10-30 | Univ Nottingham | Additive manufacturing |
CN103949654B (en) * | 2014-04-02 | 2015-12-02 | 西安交通大学 | A kind of supercritical water thermal synthesis preparation system of nano particle |
US10030292B2 (en) * | 2014-05-26 | 2018-07-24 | Hrl Laboratories, Llc | Hydride-coated microparticles and methods for making the same |
US20160339517A1 (en) * | 2015-05-21 | 2016-11-24 | Applied Materials, Inc. | Powders for additive manufacturing |
-
2018
- 2018-06-03 CN CN201880050045.6A patent/CN110997197A/en active Pending
- 2018-06-03 WO PCT/US2018/035766 patent/WO2019027563A1/en unknown
- 2018-06-03 EP EP18840807.4A patent/EP3661680A4/en active Pending
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US11154929B2 (en) | 2017-12-26 | 2021-10-26 | Daido Steel Co., Ltd. | Metal powder material |
CN115845779A (en) * | 2023-02-06 | 2023-03-28 | 河北新欣园能源股份有限公司 | Multi-functional reation kettle for chemical production |
Also Published As
Publication number | Publication date |
---|---|
WO2019027563A1 (en) | 2019-02-07 |
CN110997197A (en) | 2020-04-10 |
EP3661680A4 (en) | 2021-01-06 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
US20230415112A1 (en) | Systems and methods for nanofunctionalization of powders | |
EP3661680A1 (en) | Systems and methods for nanofunctionalization of powders | |
US11701709B2 (en) | Methods for nanofunctionalization of powders, and nanofunctionalized materials produced therefrom | |
US11919085B2 (en) | Additive manufacturing with nanofunctionalized precursors | |
US20200377983A1 (en) | Hydride-coated microparticles and methods for making the same | |
EP3661676B1 (en) | Feedstocks for additive manufacturing, and methods of using the same | |
Gu et al. | In-situ TiC particle reinforced Ti–Al matrix composites: powder preparation by mechanical alloying and selective laser melting behavior | |
EP3577245A1 (en) | Aluminum alloys with grain refiners, and methods for making and using the same | |
US20210146439A1 (en) | Functionalized aspherical powder feedstocks and methods of making the same | |
US11578389B2 (en) | Aluminum alloy feedstocks for additive manufacturing | |
KR20140125435A (en) | Method of making a metallic powder and powder compact and powder and powder compact made thereby | |
US11674204B2 (en) | Aluminum alloy feedstocks for additive manufacturing | |
EP2343387A1 (en) | Fabrication of L12 aluminum alloy tanks and other vessels by roll forming, spin forming, and friction stir welding | |
Butovsky et al. | Air stable core–shell multilayer metallic nanoparticles synthesized by RAPET: Fabrication, characterization and suggested applications | |
US20210101157A1 (en) | Spherical composite powder | |
US9994445B2 (en) | Spherical nanoparticle hydrides, and methods for making the same | |
US11396687B2 (en) | Feedstocks for additive manufacturing, and methods of using the same | |
Jennings | Hybrid powder metallurgy processing for high temperature strength Ni-base superalloy Inconel 718 |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: THE INTERNATIONAL PUBLICATION HAS BEEN MADE |
|
PUAI | Public reference made under article 153(3) epc to a published international application that has entered the european phase |
Free format text: ORIGINAL CODE: 0009012 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: REQUEST FOR EXAMINATION WAS MADE |
|
17P | Request for examination filed |
Effective date: 20200122 |
|
AK | Designated contracting states |
Kind code of ref document: A1 Designated state(s): AL AT BE BG CH CY CZ DE DK EE ES FI FR GB GR HR HU IE IS IT LI LT LU LV MC MK MT NL NO PL PT RO RS SE SI SK SM TR |
|
AX | Request for extension of the european patent |
Extension state: BA ME |
|
DAV | Request for validation of the european patent (deleted) | ||
DAX | Request for extension of the european patent (deleted) | ||
REG | Reference to a national code |
Ref country code: DE Ref legal event code: R079 Free format text: PREVIOUS MAIN CLASS: B22F0009220000 Ipc: B22F0001020000 |
|
RIN1 | Information on inventor provided before grant (corrected) |
Inventor name: MARTIN, JOHN Inventor name: YAHATA, BRENNAN Inventor name: MONE, ROBERT |
|
A4 | Supplementary search report drawn up and despatched |
Effective date: 20201204 |
|
RIC1 | Information provided on ipc code assigned before grant |
Ipc: B01J 3/04 20060101ALI20201130BHEP Ipc: B22F 1/02 20060101AFI20201130BHEP Ipc: B01J 3/02 20060101ALI20201130BHEP Ipc: B22F 3/105 20060101ALN20201130BHEP Ipc: B22F 9/02 20060101ALI20201130BHEP Ipc: C22C 1/10 20060101ALN20201130BHEP |
|
P01 | Opt-out of the competence of the unified patent court (upc) registered |
Effective date: 20230404 |
|
STAA | Information on the status of an ep patent application or granted ep patent |
Free format text: STATUS: EXAMINATION IS IN PROGRESS |