Vapor deposition process for the manufacture of coated particles

Abstract

A process for conducting vapor phase deposition is disclosed. The process separates a series of reactions through a sequence of reaction reservoirs. The reactor includes a reactive precursor reservoir beneath a powder reservoir separated by valve means. A reactive precursor is charged into the reactive precursor reservoir and a powder is charged into the powder reservoir. The pressures are adjusted so that the pressure in the reactive precursor reservoir is higher than that of the powder reservoir. The valve means is opened, and the vapor phase reactant fluidized the powder and coats its surface. The powder falls into the reactive precursor reservoir. The apparatus permits vapor phase deposition processes to be performed semi-continuously.

1 . An apparatus for coating particles by atomic layer deposition comprising:
 (a) a first reactor capable of bringing particles in contact with a first reactive gas,   (b) a second reactor capable of bringing particles in contact with a second reactive gas, and   (c) at least one separating device for separating particles from a first reactive gas or a second reactive gas located between the first reactor and the second reactor,
 wherein the first and the second reactor are separated by a valve assembly comprising a first gas lock and a second gas lock and the particles can be conveyed from the first reactor through the first gas lock to the second reactor or to a separating device (c) and at the same time the particles can be conveyed from the second reactor through the second gas lock to the first reactor or to a separating device (c). 
   
     
     
         2 . The apparatus according to  claim 1 , wherein the first reactor is equipped with a first gas inlet valve, which is equipped with a first gauge to measure the flow rate and means to control the flow rate of the first reactive gas through the first gas inlet valve, and wherein the second reactor is equipped with a second gas inlet valve, which is equipped with a second gauge to measure the flow rate and means to control the flow rate of the second reactive gas through the second gas inlet valve. 
     
     
         3 . The apparatus according to  claim 1 , wherein the first reactor has a geometry comprising a first diameter, a conical section with inwardly slanting walls that introduces a restricted cross-section in the direction of the flow of particles, and a connection to a first gas lock, wherein if said first gas lock valve is:
 a. in a closed position, is capable of maintaining the pressure within the first reactor;   b. in an open position, is capable of facilitating the transfer of the particles out of the first reactor.   
     
     
         4 . An apparatus for coating particles by atomic layer deposition comprising:
 a. a first reactor capable of bringing the particles in contact with a first reactive gas having a first reactor particle inlet and a first reactor particle outlet;   b. a second reactor capable of bringing the particles in contact with a second reactive gas having a second reactor particle inlet and a second reactor particle outlet;   c. a first separation device capable of separating the particles from a first reactive gas, having a first separation device particle-gas inlet, a first separation device gas outlet, and a first separation device particle outlet;   d. a second separation device capable of separating the particles from a second reactive gas, having a second separation device particle-gas inlet, a second separation device gas outlet, and a second separation device particle outlet;   e. a first constricted flow path comprising a first valve assembly connected to the first reactor particle inlet, capable of controlling the conveying of the particles into the first reactor;   f. a second constricted flow path comprising a second valve assembly capable of controlling the conveying of the particles from the first reactor particle outlet through the second valve assembly to the second reactor, or to a first separation device;   g. a third constricted flow path comprising a third valve assembly capable of controlling the conveying of the particles from the second reactor particle outlet through the third valve, or to a first separation device.   
     
     
         5 . The apparatus of  claim 4 , further comprising:
 h. A first reactive gas inlet valve assembly in fluid communication with both the first reactor and a first reactive gas feed system, said first reactive gas inlet valve assembly comprising: a first reactive gas inlet valve, a first reactive gas pressure meter and a first reactive gas flow meter, wherein if said first reactive gas inlet valve is:
 1. in an open position, is capable of monitoring and controlling the pressure of the first reactive gas in the first reactor, and 
 2. in a closed position, is capable of maintaining the pressure of the first reactive gas in the first reactor; 
   i. A second reactive gas inlet valve assembly in fluid communication with both the second reactor and a second reactive gas feed system, said second reactive gas inlet valve assembly comprising: a second reactive gas inlet valve, a second reactive gas pressure meter and a second reactive gas flow meter, wherein if the second reactive gas inlet valve is:
 1. in an open position, is capable of monitoring and controlling the pressure of the second reactive gas in the second reactor, and 
 2. in a closed position, is capable of maintaining the pressure of the second reactive gas in the second reactor; 
   
     
     
         6 . The apparatus of  claim 4 , further comprising a first particle conveyor having a first particle conveyor inlet and a first particle conveyor outlet, wherein either:
 the first particle conveyor inlet is in fluid communication with the first separation device particle outlet, and the first particle conveyor outlet is in fluid communication with the second valve assembly; or   the first particle conveyor inlet is in fluid communication with the second valve assembly, and the first particle conveyor outlet is in fluid communication with the first separation device particle-gas inlet.   
     
     
         7 . The apparatus of  claim 4 , wherein the first separation device gas-particle inlet and the first separation device particle outlet are each in fluid communication with the first reactor. 
     
     
         8 . The apparatus of  claim 7 , wherein the second separation device gas-particle inlet and the second separation device particle outlet are each in fluid communication with the second reactor. 
     
     
         9 . The apparatus of  claim 4 , wherein the particles are selected from particles for lithium ion batteries, particles or substrates for catalysts, particles of titanium dioxide, ultra-fine metal particles, air-sensitive particles, moisture-sensitive particles, and phosphor particles. 
     
     
         10 . The apparatus of  claim 4 , capable of applying: i) oxide coatings including aluminum oxide, silicon oxide, zinc oxide, zirconium oxide, titanium oxide, boron oxide, yttria, zinc oxide and magnesium oxide; ii) nitride coatings including silicon nitride, boron nitride and aluminum nitride; iii) sulfide coatings including gallium sulfide, tungsten sulfide and molybdenum sulfide; iv) inorganic phosphides; v) metal coatings including cobalt, palladium, platinum, zinc, rhenium, molybdenum, antimony, selenium, thallium, chromium; platinum, ruthenium, iridium, germanium and tungsten; and vi) rare earth elements. 
     
     
         11 . The apparatus of  claim 4 , further capable of coating particles by molecular layer deposition, and capable of applying: vii) organic coatings; and viii) hybrid inorganic-organic coatings. 
     
     
         12 . The apparatus of  claim 4 , capable of coating particles at a rate of at least 0.8 kilograms per hour. 
     
     
         13 . An apparatus for coating particles having a first particle batch and a second particle batch by atomic layer deposition comprising:
 a. a first reactor capable of bringing the first particle batch in contact with a first reactive gas having a first reactor particle inlet and a first reactor particle outlet;   b. a second reactor capable of bringing the second particle batch in contact with a second reactive gas having a second reactor particle inlet and a second reactor particle outlet;   c. a first separation device capable of separating the first particle batch from a first reactive gas, having a first separation device particle-gas inlet, a first separation device gas outlet, and a first separation device particle outlet;   d. a second separation device capable of separating the second particle batch from a second reactive gas, having a second separation device particle-gas inlet, a second separation device gas outlet, and a second separation device particle outlet;   e. a first constricted flow path comprising a first valve assembly connected to the first reactor particle inlet, capable of controlling the conveying of the first particle batch into the first reactor;   f. a second constricted flow path comprising a second valve assembly capable of controlling the conveying of the first particle batch from the first reactor particle outlet through the second valve assembly to the second reactor, or to a first separation device;   g. a third constricted flow path comprising a third valve assembly capable of controlling the conveying of the second particle batch from the second reactor particle outlet through the third valve, or to the second separation device.   wherein the apparatus is capable of saturating the entire surface of the first particle batch with a first reactive gas and saturating the entire surface of the second particle batch with a second reactive gas simultaneously and via computer control.   
     
     
         14 . The apparatus of  claim 13 , further comprising:
 h. A first reactive gas inlet valve assembly in fluid communication with both the first reactor and a first reactive gas feed system, said first reactive gas inlet valve assembly comprising: a first reactive gas inlet valve, a first reactive gas pressure meter and a first reactive gas flow meter, wherein if said first reactive gas inlet valve is:
 1. in an open position, is capable of monitoring and controlling the pressure of the first reactive gas in the first reactor, and 
 2. in a closed position, is capable of maintaining the pressure of the first reactive gas in the first reactor; 
   j. A second reactive gas inlet valve assembly in fluid communication with both the second reactor and a second reactive gas feed system, said second reactive gas inlet valve assembly comprising: a second reactive gas inlet valve, a second reactive gas pressure meter and a second reactive gas flow meter, wherein if the second reactive gas inlet valve is:
 1. in an open position, is capable of monitoring and controlling the pressure of the second reactive gas in the second reactor, and 
 2. in a closed position, is capable of maintaining the pressure of the second reactive gas in the second reactor; 
   
     
     
         15 . The apparatus of  claim 13 , further comprising a first particle conveyor having a first particle conveyor inlet and a first particle conveyor outlet, wherein:
 the first particle conveyor inlet is in fluid communication with the first separation device particle outlet, and the first particle conveyor outlet is in fluid communication with the second valve assembly, or   the first particle conveyor inlet is in fluid communication with the second valve assembly, and the first particle conveyor outlet is in fluid communication with the first separation device particle-gas inlet, or   the first particle conveyor inlet is in fluid communication with the second valve assembly and the first particle conveyor outlet is in fluid communication with the second reactor.   
     
     
         16 . The apparatus of  claim 13 , wherein the first separation device gas-particle inlet and the first separation device particle outlet are each in fluid communication with the first reactor. 
     
     
         17 . The apparatus of  claim 16 , wherein the second separation device gas-particle inlet and the second separation device particle outlet are each in fluid communication with the second reactor. 
     
     
         18 . The apparatus of  claim 13 , wherein the particles are selected from particles for lithium ion batteries, particles or substrates for catalysts, particles of titanium dioxide, ultra-fine metal particles, air-sensitive particles, moisture-sensitive particles, and phosphor particles. 
     
     
         19 . The apparatus of  claim 13 , capable of applying: i) oxide coatings including aluminum oxide, silicon oxide, zinc oxide, zirconium oxide, titanium oxide, boron oxide, yttria, zinc oxide and magnesium oxide; ii) nitride coatings including silicon nitride, boron nitride and aluminum nitride; iii) sulfide coatings including gallium sulfide, tungsten sulfide and molybdenum sulfide; iv) inorganic phosphides; v) metal coatings including cobalt, palladium, platinum, zinc, rhenium, molybdenum, antimony, selenium, thallium, chromium; platinum, ruthenium, iridium, germanium and tungsten and vi) rare earth elements. 
     
     
         20 . The apparatus of  claim 13 , further capable of coating particles by molecular layer deposition, and capable of applying: vii) organic coatings; and viii) hybrid inorganic-organic coatings. 
     
     
         21 . The apparatus of  claim 13 , capable of coating particles at a rate of at least 0.8 kilograms per hour.