Method for the production of multiphase composite materials using microwave plasma process
Disclosed herein is a method to produce multiphase composite materials directly from solution precursor droplets by a fast pyrolysis process using a microwave plasma embodiment containing a microwave generating source, a dielectric plasma torch, and a droplet maker. Here, using homogenous solution precursors, droplets are generated with a narrow size distribution, and are injected and introduced into the microwave plasma torch with generally uniform thermal path. The generally uniform thermal path in the torch is achieved by axial injection of droplets into an axisymmetric hot zone with laminar flows. Upon exposing to high temperature within the plasma with controlled residence time, the droplets are pyrolyzed and converted into particles by quenching with a controlled rate of the exhaust gas in a gas chamber. The particles generated have generally uniform sizes and uniform thermal history, and can be used for a variety of applications.
1. A method of making particles using a microwave generated plasma comprising:
a. preparing a salt solution in water, in organic solvent, or in a mixture of water and organic solvent;
b. generating precursor droplets from said salt solution using a feed injection device;
c. introducing axially said precursor droplets into a microwave plasma torch;
d. entraining said precursor droplets using at least two concentric laminar gas flows towards a microwave generated plasma;
e. exposing said precursor droplets to high temperature within said microwave generated plasma;
f. controlling residence time of said precursor droplets in said microwave generated plasma;
g. controlling quenching rates of an exhaust gas of said microwave generated plasma in a gas chamber;
h. filtering the exhaust gas of said microwave generated plasma; and
i. extracting particles from said exhaust gas.
2. The method of claim 1 , wherein said step of preparing a salt solution is prepared by further adding an acid to water, organic solvent, or to a mixture of water and organic solvent.
3. The method of claim 1 , wherein said step of preparing a salt solution is prepared by combining at least a first solution and a second solution.
4. The method of claim 3 , further comprising preparing said first solution by:
mixing water and organic solvent;
adding an acid to water; or
adding an acid to a mixture of water and organic solvent.
5. The method of claim 3 , further comprising preparing said second solution by:
dissolving at least one salt in water; or
dissolving at least one salt in mixture of water and organic solvent.
6. The method of claim 3 , further comprising preparing said first solution by:
mixing water and ethylene glycol;
adding citric acid to water; or
adding citric acid to a mixture of water and ethylene glycol.
7. The method of claim 1 , wherein said step of preparing a salt solution is prepared in a mixture of water and organic solvent and further selecting the organic solvent from the group consisting of ethanol, methanol, 1-propanol, 2-propanol, tetrahydrofuran, and a combination thereof.
8. The method of claim 1 , wherein said salt solution includes a salt selected from the group consisting of cations of lithium, sodium, potassium, rubidium, magnesium, calcium, strontium, barium, scandium, yttrium, titanium, vanadium, chromium, manganese, iron, cobalt, nickel, copper, zinc, zirconium, niobium, molybdenum, technetium, ruthenium, rhodium, palladium, silver, cadmium, hafnium, tantalum, tungsten, rhenium, osmium, iridium, platinum, gold, aluminum, gallium, indium, tin, thallium, lead, bismuth, lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, thorium, boron, silicon, germanium, arsenic, antimony, tellurium, carbon, phosphorus, sulfur, selenium, and combinations thereof.
9. The method of claim 1 , wherein said step of preparing a salt solution comprises dissolving salts comprising cations of:
aluminum;
yttrium, scandium, or combinations thereof; and
dopants selected from the group consisting of lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, and a combination thereof.
10. The method of claim 1 , wherein said step of preparing a salt solution comprises dissolving salts comprising cations of:
aluminum, zirconium, silicon, magnesium, and manganese, or combinations thereof; and
doping transition metals selected from the group consisting of palladium, platinum, nickel, silver, gold, ruthenium, rhodium, vanadium, molybdenum, cobalt, tungsten, and any combination thereof.
11. The method of claim 1 , wherein said step of preparing a salt solution comprises dissolving salts comprising cations of magnesium and yttrium.
12. The method of claim 1 , wherein said step of preparing a salt solution comprises dissolving salts comprising cations of magnesium and aluminum.
13. The method of claim 1 , wherein said step of preparing a salt solution comprises dissolving salts comprising cations of lanthanum; magnesium; and aluminum.
14. The method of claim 1 , wherein said step of preparing a salt solution comprises dissolving salts comprising cations of:
zirconium; and
yttrium or samarium.
15. The method of claim 1 , wherein said step of preparing a salt solution comprises dissolving salts selected from the group consisting of nitrate, acetate, citrate, sulfate, carbonate, chloride, phosphate, alkoxide, atrane, tetraethyl, orthosilicate, metallic borohydride, and a combination thereof.
16. The method of claim 1 , wherein said at least two concentric laminar flows comprise flows of gas selected from the group consisting of air, oxygen, argon, methane, ammonia, nitrogen, and a combination thereof.
17. The method of claim 1 , wherein said step of controlling quenching rates is further adjusted by selecting a rate no less than 10 3 Kelvin per second (K/s) to no more than 10 6 K/s.
18. The method of claim 17 , wherein controlling quenching rates comprises controlling quenching rates of an exhaust gas of said microwave generated plasma in a gas chamber with controllable atmosphere.