Method of fabricating tungsten scandate nano-composite powder for cathodes
US-2017358419-A1 · Dec 14, 2017 · US
US10497530B2 · US · B2
| Field | Value |
|---|---|
| Publication number | US-10497530-B2 |
| Application number | US-201615093853-A |
| Country | US |
| Kind code | B2 |
| Filing date | Apr 8, 2016 |
| Priority date | Apr 10, 2015 |
| Publication date | Dec 3, 2019 |
| Grant date | Dec 3, 2019 |
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A thermionic dispenser cathode having a refractory metal matrix with scandium and barium compounds in contact with the metal matrix and methods for forming the same. The invention utilizes atomic layer deposition (ALD) to form a nanoscale, uniform, conformal distribution of a scandium compound on tungsten surfaces and further utilizes in situ high pressure consolidation/impregnation to enhance impregnation of a BaO—CaO—Al2O3 based emissive mixture into the scandate-coated tungsten matrix or to sinter a tungsten/scandate/barium composite structure. The result is a tungsten-scandate thermionic cathode having improved emission.
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What is claimed is: 1. A process for making a thermionic dispenser cathode from a scandium-coated powder, the process including: providing a starting powder comprising particles of a refractory metal and/or metal alloy; placing the starting powder inside a furnace having a controlled atmosphere and heating the starting powder in the flow of hydrogen or hydrogen/inert gas mixture to reduce surface oxides to produce a cleaned starting powder; without exposing the cleaned starting particle to an external atmosphere, placing the cleaned starting powder inside a particle atomic layer deposition (ALD) reactor and controllably depositing a conformal nanometer-scale film of a scandium compound on the surface of all particles of the starting powder to produce a scandium-coated (Sc-coated) powder comprising the particles of the starting powder with a conformal nanometer-scale scandium film having a predetermined thickness uniformly deposited on all of the particles thereof; placing the Sc-coated powder in contact with an emissive mixture; without exposing the Sc-coated powder contacted with the emissive mixture to the air, applying a predetermined pressure P to the Sc-coated powder at room temperature to form a porous compact from the Sc-coated powder, wherein the pressure P is sufficient to break the scandium film on the surface of the Sc-coated particles so that the particles make electrical contact with one another but not high enough to cause the compact to lose porosity, the compact being in contact with the emissive mixture; and without exposing the porous compact in contact with the emissive mixture to air, heating the compact and the emissive mixture to a predetermined temperature T greater than a melting point of the emissive mixture so that the emissive mixture becomes a molten emissive mixture that impregnates the porous compact; wherein the impregnated compact forms the cathode. 2. The process according to claim 1 , wherein the refractory metal and/or metal alloy is tungsten. 3. The process according to claim 1 , wherein the scandium compound is scandium oxide. 4. The process according to claim 1 , wherein the emissive mixture is barium-calcium-aluminate. 5. The process according to claim 1 , wherein the emissive mixture is a barium compound. 6. The process according to claim 1 , wherein the emissive mixture comprises barium oxide calcium oxide, or aluminum oxide. 7. The process according to claim 1 , wherein the pressure P is between about 0.1 and 5 GPa. 8. The process according to claim 1 , wherein the temperature T is between 1500° C. and 2100° C. 9. A process for making a thermionic dispenser cathode from a scandium- and barium-coated powder, the process including: providing a starting powder comprising particles of a refractory metal and/or metal alloy; placing the starting powder inside a furnace having a controlled atmosphere and heating the starting powder in the flow of hydrogen or hydrogen/inert gas mixture to reduce surface oxides to produce a cleaned starting powder; without exposing the cleaned starting powder to an external atmosphere, placing the cleaned starting powder inside a particle atomic layer deposition (ALD) reactor and controllably depositing a conformal nanometer-scale film of a scandium compound on the surface of all particles of the starting powder to produce a scandium-coated (Sc-coated) powder comprising the particles of the starting powder with a conformal nanometer-scale scandium film having a predetermined thickness uniformly deposited on all of the particles thereof; with the Sc-coated powder still in the ALD reactor and without exposing the Sc-coated powder to the atmosphere, further controllably depositing a conformal layer of a barium compound on the Sc-coated powder to form a scandium- and barium-coated (Sc/Ba-coated) powder; without exposing the Sc/Ba-coated powder to the atmosphere, applying a predetermined pressure P to the Sc/Ba-coated powder at room temperature to form a porous compact from the Sc/Ba-coated powder, wherein P is sufficient to break the Sc/Ba film on the surface of the coated particles so that the particles make electrical contact with one another but not high enough to cause the compact to lose porosity; and without exposing the porous compact to air, heating the porous compact to a predetermined temperature T at pressure P to sinter the porous compact to a dense compact, wherein the dense compact does not have a connected porosity or a porosity of less than 15%; wherein the dense compact forms the cathode. 10. The process according to claim 9 , wherein the refractory metal and/or metal alloy is tungsten. 11. The process according to claim 9 , wherein the scandium compound is scandium oxide. 12. The process according to claim 9 , wherein the barium compound is barium-calcium-aluminate. 13. The process according to claim 9 , wherein the pressure P is between about 0.1 and 5 GPa. 14. The process according to claim 9 , wherein the temperature T is between 800° C. and 2100° C.
Dispenser-type cathodes, e.g. L-cathode · CPC title
with alkaline-earth metal oxides, or such oxides used in conjunction with reducing agents, as an emissive material · CPC title
Impregnating {(making ferrous alloys by impregnation C22C33/0242)} · CPC title
Aspects linked to processes or compositions used in powder metallurgy · CPC title
Metallic particles coated with a non-metal (coated with lubricating or binding agents or with organic material B22F1/10) · CPC title
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