JP2016522734A - High-throughput particle production using a plasma system - Google Patents

Abstract

The present disclosure relates to nanoparticle production systems and methods of using the systems. The nanoparticle production system includes a plasma including a male electrode, a female electrode, and a working gas source configured to deliver a working gas in a vortex spiral direction across the plasma generation region. Includes cancer. The system also includes a continuous delivery system, a quench chamber, a cooling conduit that includes a laminar flow disruptor, a system overpressure module, and a conditioned fluid purification and recirculation system. The continuous feed system is configured to feed material into the plasma gun at a rate of at least 9 grams / minute.

Description

(Cross-reference to related applications)
This application is based on US patent application No. 61 / 784,299, filed Mar. 14, 2013, US patent application No. 61 / 864,350, filed Aug. 9, 2013, October 2013. US Patent Application No. 61 / 885,988 filed on the 2nd, US Patent Application No. 61 / 885,990 filed on the 2nd October 2013, US Patent filed on the 2nd October 2013 No. 61 / 885,996, and US Patent Application No. 61 / 885,998 filed Oct. 2, 2013, claiming priority benefit. The entire contents of those applications are hereby incorporated by reference herein.

(Field of Invention)
The present invention relates to systems and methods for providing high throughput particle production using plasma.

(Background of the Invention)
Nanoparticles can be formed using a plasma production system in which one or more raw materials are fed into a plasma gun that uses a working gas to generate a plasma. The plasma evaporates the raw material, which is then condensed and forms nanoparticles in a quenching reaction. The nanoparticles can then be collected and used for various industrial applications.

  Typical plasma-based particle production systems are limited in their ability to remain in continuous operation with consistent material throughput and are typically based on experimental and pilot plant scale designs. These systems are typically very limited in mass / volume throughput. This makes inefficient industrial scale production of consistent quality and size nanoparticles.

(Summary of the Invention)
Described are nanoparticle production systems, devices used in such systems, and methods of using the systems and devices. The nanoparticle production system includes a male electrode, a female electrode, and a working gas source configured to deliver a working gas in a spiral flow direction across the plasma generation region. May be included. The system may also include one or more of a continuous feed system, a quench chamber, a cooling conduit including a laminar flow disruptor, a system overpressure module, and a conditioned fluid purification and recirculation system. This system incorporating various combinations of these features is also recalled, and in some cases, a system having a combination of these features is produced, improving the length of time that the system can be operated continuously. It provides separate technical advantages, such as improved particle quality or quantity, and / or improved production system efficiency. Methods of producing nanoparticles using these systems also form part of the proposal.

  In some embodiments, the nanoparticle production system includes a plasma gun and a continuous delivery system configured to deliver material into the plasma gun at a rate of at least 9 grams / minute.

  In any of the embodiments, the continuous feed system may be configured to feed material to the plasma gun for at least 336 hours without clogging. In any of the embodiments, the continuous feed system may include a plurality of material feed supply channels for supplying raw material to the plasma gun. In any of the embodiments, the continuous feed system may include a reciprocating member for continuously sweeping the material feed supply channel during operation of the nanoparticle production system. In any of the embodiments, the reciprocating member may reciprocate at a rate of at least 2 times / second.

  In any of the embodiments, the continuous delivery system may include a pulsed gas spray to continuously sweep the material delivery supply channel during operation of the nanoparticle production system.

  In any of the embodiments, the plasma gun has a working gas flow in a spiral flow direction across the plasma generation region formed between the male electrode, the female electrode, and the male electrode and the female electrode. And a working gas source configured to deliver to.

  In any of the embodiments, the working gas supply may include an injection ring that is positioned in front of the plasma generation region and generates a vortex spiral flow direction. In any of the embodiments, the injection ring may include a plurality of injection ports. In any of the embodiments, the injection port may be arranged in an annular form around the male electrode. In any of the embodiments, the injection port may be angled toward the male electrode.

  In any of the embodiments, the injection port may be angled away from the male electrode. In any of the embodiments, the nanoproduction system may be operable for at least 336 hours without replacement of the male or female electrode.

  In any of the embodiments, the nanoparticle production system may further include a quench chamber positioned after the plasma gun and including at least one reaction mixture input and at least one conditioned fluid input. In any of the embodiments, the quench chamber may have a frustoconical shape and may be configured to generate turbulence with a Ray nozzle coefficient greater than 1000 during operation.

  Any of the embodiments may further include a cooling conduit configured to conduct nanoparticles entrained in the conditioned fluid stream from the quench chamber to the collector. In any of the embodiments, the cooling conduit may include a laminar flow disruptor. In any of the embodiments, the laminar flow disruptor may include a blade, baffle, helical screw, ridge, or bump. In any of the embodiments, the particle production system may be configured to operate continuously for at least 6 hours without clogging in the cooling conduit. Any of the embodiments may further include a cooling conduit configured to conduct nanoparticles entrained in the conditioned fluid stream from the quench chamber to the collector. In any of the embodiments, the cooling conduit may include a laminar flow disruptor. In any of the embodiments, the laminar flow disruptor may include a blade, baffle, helical screw, ridge, or bump. In any of the embodiments, the particle production system may be configured to operate continuously for at least 336 hours without clogging in the cooling conduit.

  Any of the embodiments may further include a system overpressure module that maintains a pressure in the system above the measured ambient pressure. In any of the embodiments, the pressure in the system may be maintained at a pressure that is at least one inch of water above the measured ambient pressure. Any of the embodiments may further include a system overpressure module that maintains a pressure in the system above the measured ambient pressure.

  Any of the embodiments may further include a conditioned fluid purification and recirculation system. In any of the embodiments, at least 80% of the conditioned fluid introduced into the nanoparticle production system may be purified and recycled.

  In some embodiments, the nanoparticle production system vortexes a working gas across a plasma generation region formed between a male electrode, a female electrode, and a male electrode and a female electrode. A plasma gun including a working gas source configured to deliver in a flow direction; and a continuous feed system configured to deliver material into the plasma gun at a rate of at least 9 grams / minute; A quench chamber positioned after the plasma gun and comprising at least one reaction mixture input and at least one conditioned fluid input and configured to conduct nanoparticles entrained in the conditioned fluid stream from the quench chamber to the collector A cooling conduit comprising a laminar flow disruptor and a system overpressure module for maintaining a pressure in the system above the measured ambient pressure. And a fluid purification and recirculation system.

FIG. 1 is a schematic diagram of one embodiment of a plasma system useful for producing nanoparticles. FIG. 2A is a schematic diagram of one embodiment of a plasma gun with a material delivery port. FIG. 2B is a schematic illustration of one embodiment of a plasma gun with a face plate and a cooling ring. FIG. 2C is a schematic illustration of an alternative embodiment of a plasma gun with a plasma gun faceplate and cooling ring. FIG. 2D is a schematic illustration of a tangential view of an embodiment of a plasma gun with the plasma gun faceplate and cooling ring illustrated in FIG. 2B. FIG. 2E is a schematic illustration of one embodiment of a plasma gun with a reduced plasma gun faceplate, cooling ring, and a wider, refractory conductive metal lined plasma channel. 2F is a schematic illustration of a tangential view of an embodiment of a plasma gun with a reduced plasma gun faceplate, a cooling ring, and a wider, heat resistant conductive metal lined plasma channel illustrated in FIG. 2E. is there. FIG. 3A is a schematic illustration of one embodiment of a plasma gun useful for a high-throughput particle production system with a working gas injection ring and alternating material injection ports that allow continuous material delivery. FIG. 3B is a schematic illustration of one embodiment of a plasma gun useful for a high-throughput particle production system with a working gas injection ring and a reciprocating plunger device that allows continuous material delivery. FIG. 3C is a schematic illustration of one embodiment of a plasma gun useful for a high throughput particle production system with a working gas injection ring and a pulsed air atomization system that allows continuous material delivery. FIG. 3D includes a reduced plasma gun faceplate, cooling ring, wider, refractory metal-lined plasma channel, working gas injection ring, and alternating material injection port that allow continuous material delivery. 1 is a schematic illustration of one embodiment of a plasma gun useful for a high throughput particle production system. FIG. 3E includes a reduced plasma gun faceplate, cooling ring, wider, refractory conductive metal lined plasma channel, working gas injection ring, and reciprocating plunger device that allow continuous material delivery. 1 is a schematic illustration of one embodiment of a plasma gun useful for a high throughput particle production system. FIG. 3F involves a reduced plasma gun faceplate, cooling ring, wider, refractory conductive metal lined plasma channel, working gas injection ring, and pulsed air atomization system that allows continuous material delivery. 1 is a schematic illustration of one embodiment of a plasma gun useful for a high throughput particle production system. FIG. 4A is a schematic diagram of one embodiment of a high throughput particle production system with a super turbulent quench chamber and a turbulence induced spray. FIG. 4B is a schematic illustration of an alternative embodiment of a high throughput particle production system with a super turbulent quench chamber and a turbulence induced spray, where the turbulence induced spray is interconnected in a ring structure. FIG. 5 is a detailed schematic diagram of the turbulence inducing spray interconnected in the ring structure illustrated in FIG. 4B. FIG. 6A is a schematic diagram of one embodiment of a high throughput particle production system with a laminar flow disruptor. FIG. 6B is a schematic diagram of an alternative embodiment of a high throughput particle production system with a laminar flow disruptor. FIG. 6C is a schematic illustration of an alternative embodiment of a high throughput particle production system with a laminar flow disruptor using air atomization. FIG. 6D is a schematic illustration of an alternative embodiment of a high throughput particle production system with a laminar flow disruptor that uses rotating axially arranged rods. FIG. 7 is a tangential schematic diagram of one embodiment of a laminar flow disruptor using the rotating axially arranged rods illustrated in FIG. 6D. FIG. 8 is a schematic illustration of one embodiment of a high throughput particle production system with a gas delivery system with constant overpressure. FIG. 9 is a schematic diagram of one embodiment of a high throughput particle production system with a conditioned fluid purification and recirculation system. FIG. 10 is a schematic illustration of one embodiment of a high throughput particle production system with a conditioned fluid purification and recirculation system integrated into a system overpressure module of a gas delivery system with constant overpressure. FIG. 11 is a schematic diagram of one embodiment of a high-throughput particle production system with a filter back pulse system useful for removing clogging of filter elements in the collection device.

(Detailed description of the invention)
A typical nanoparticle production system feeds material into a plasma stream, thereby evaporating the material, and the reactive plasma mixture produced cools the nanoparticles and composites or “nano-nano”. On-nano) "nanoparticles can be generated by allowing them to solidify. The particles can then be collected for use in various applications. Preferred nanoparticles and “nano-on-nano” particles are described in US application Ser. No. 13 / 801,726, the description of which is hereby incorporated by reference in its entirety.

  The present disclosure refers to both particles and powders. These two terms are equivalent, but the singular “powder” refers to a collection of particles. The present invention can be applied to a wide variety of powders and particles. The terms “nanoparticle” and “nanosize particle” generally refer to particles of about nanometer diameter, typically about 0.5 nm to 500 nm, about 1 nm to 500 nm, about 1 nm to 100 nm, or about 1 nm to 50 nm. It is understood by those skilled in the art to include. Preferably, the nanoparticles have an average particle size of less than 250 nanometers and an aspect ratio of 1 to 1 million. In some embodiments, the nanoparticles have an average particle size of about 50 nm or less, about 30 nm or less, or about 20 nm or less. In additional embodiments, the nanoparticles have an average diameter of about 50 nm or less, about 30 nm or less, or about 20 nm or less. The aspect ratio of the particles, defined as the longest dimension of the particles divided by the shortest dimension of the particles, is preferably 1-100, more preferably 1-10, and even more preferably 1-2. “Granularity” is measured using the ASTM (American Society for Testing and Materials) standard (see ASTM E112-10). When calculating the diameter of a particle, the average of its longest and shortest dimensions is determined. Thus, the diameter of an oval particle with a major axis of 20 nm and a minor axis of 10 nm will be 15 nm. The average diameter of a collection of particles is the average of the diameters of individual particles and can be measured by various techniques known to those skilled in the art.

  In additional embodiments, the nanoparticles have a particle size of about 50 nm or less, about 30 nm or less, or about 20 nm or less. In additional embodiments, the nanoparticles have a diameter of about 50 nm or less, about 30 nm or less, or about 20 nm or less.

  Composite nanoparticles are formed by the joining of two different nanoparticles. This binding can occur during the quench phase of the nanophase production method. For example, the catalyst may comprise catalyst nanoparticles attached to supporting nanoparticles to form “nano-on-nano” composite nanoparticles. A plurality of nano-on nanoparticles can then be combined with micron-sized carrier particles to form composite micro / nanoparticles, ie, microparticles carrying composite nanoparticles.

  As shown in FIG. 1, a plasma system 100 useful for producing nanoparticles includes a plasma gun 102, a material input delivery system 104, a quench chamber 106 fluidly connected to a cooling conduit 108, Output collection system 110. A working gas 112 flows through the plasma gun 102 and generates a plasma, while a conditioned fluid 114 flows into the gun box 116 and then into the quench chamber 106. A negative pressure can be applied to the collection end of the plasma production system using a vacuum or blower 118 to provide a directional flow of conditioned fluid and material output.

  FIG. 2A illustrates an embodiment of a plasma gun that can be used for particle production. The plasma gun 200 includes a male electrode 202 and a female electrode 204, and an internal chamber is formed between the male electrode 202 and the female electrode 204. The internal chamber includes an inflow region 206 at one end and a plasma region 208 at the opposite end. In some embodiments, the inflow region 206 has a cylindrical shape while the plasma region 208 has a frustoconical shape. The internal chamber is configured to introduce working gas into its inflow region 206 and then flow into the plasma region 208. In some embodiments, the working gas is an inert gas, such as argon. In some embodiments, hydrogen or other gas may be added to argon to reduce nanoparticle oxidation.

  For example, in some embodiments, the working gas is a mixture of argon and hydrogen in a ratio of 30: 1 to 3: 1. In some embodiments, the working gas is a mixture of argon and hydrogen in a 20: 1 ratio. In some embodiments, the working gas is a mixture of argon and hydrogen in a 12: 1 ratio. In some embodiments, the working gas is a mixture of argon and hydrogen in an 8: 1 ratio. In some embodiments, the working gas is a mixture of argon and hydrogen in a 5: 1 ratio. The gas inlet 210 is configured to supply working gas to the inflow region 206. During operation of the high throughput plasma-based particle production system, working gas flows through the inflow region 206, into the plasma region 208, and out from the outlet 212. A power supply is connected to the male electrode 202 and female electrode 204 to pass power by passing current across the gap between the male electrode 202 and female electrode 204 in the plasma region 208. Delivered through plasma gun 200. A current arc across the gap in the plasma region 208 excites the working gas and creates a plasma stream that flows out of the outlet 212.

  As the evaporated material is exhausted from the plasma gun, radiant heat can damage a portion of the plasma gun. As illustrated in FIGS. 2B-D, a cooling ring 218 is positioned within the female electrode 204 and is annularly disposed about the outlet 212 to provide heat to the female electrode 204 and other plasma gun 200 components. Induced damage can be prevented or slowed down. A cooling fluid, such as water, can be recirculated through the cooling ring 218 to dissipate some of the heat generated by the plasma during system operation. A face plate 220 can be joined to the cooling ring. The face plate 220 may be disposed on the outer surface of the plasma gun 200 and used to hold the female electrode 204 in place and seal the cooling ring 218. In FIG. 2D, the dashed line represents the cooling ring 218, which is covered by the face plate 220. The cooling fluid is circulated through the cooling ring 218 by flowing in through the cooling ring inflow port 234 and out through the cooling ring outflow port 236. The cooling fluid may be recirculated using a pump or otherwise arranged. As the plasma is generated in the plasma region 208 and travels through the cylindrical channel 209 in the female electrode 204 and exits through the outlet, the radiant heat generated by the plasma can be dissipated by the cooling fluid.

  A material injection port 214 can be disposed on the female electrode 204 that connects the material feed channel 216 to the cylindrical channel 209. The raw material can be fed through the material feed channel 216 into the cylindrical channel 209 and evaporated by the plasma before flowing from the outlet 212 into the quench chamber. Particle nucleation and surface growth occurs in the cylindrical channel 209 immediately after energy delivery, and the particles continue to grow in size in the quench chamber. The particles are cooled in the quench chamber and cooling conduit before being collected by the collection system. After particle collection, the conditioned fluid is generally vented into the environment or otherwise disposed.

  For cost effective large scale production of nanoparticles, high material throughput and continuous operation of the nanoparticle production system is preferred. Previous plasma-based nanoparticle production systems suffered from frequent shutdowns to clear clogged channels and replace worn parts. For example, the heat of the plasma gun frequently melts the raw material, clogs the material delivery channel, and the clogging can only be removed if the system is shut down. The plasma gun electrode pits during operation and the system will need to be shut down to replace these parts. The plasma gun faceplate can also melt during continuous operation, allowing cooling fluid to leak out of the cooling ring, resulting in system shutdown to replace the faceplate. Particles may accumulate along the walls of the cooling conduit and the system will need to be shut down to clean the cooling conduit. Furthermore, the nanoparticle size was inconsistent and difficult to control due to variations in system pressure and material flow rate. For example, if the pressure in the quench chamber is below ambient pressure, impurities can leak into the system and degrade the quality of the produced nanoparticles. In addition, uncontrolled cooling and material flow rates within the quench chamber led to inconsistent sized particles. Another concern was that disposal of spent conditioned fluid was not cost effective for large scale production. Such obstacles interfere with average throughput speed, cost effectiveness, and consistency of particles produced by plasma-based nanoparticle production systems.

  The described systems, devices, and methods reduce the inoperability of the system, produce a larger amount of more consistent throughput, and use a high-throughput particle production system to produce more consistent nanoparticles To do. Such high throughput systems, devices, and methods produce a continuous and consistent flow by reducing outages and variability in the system. The high throughput particle production system has at least 6 grams, at least 12 hours, at least 24 hours, with a material throughput of at least 9 grams / minute, preferably 30 grams / minute, more preferably 60 grams / minute, It can remain operational for at least 48 hours, at least 72 hours (3 days), at least 336 hours (14 days), at least 672 hours (28 days), or at least 1344 hours (56 days).

  Particle production system throughput depends on a constant material flow. Slow or inconsistent material flows cause system congestion and result in uneven particle size distribution. The described system, apparatus, and method include a continuous input raw material flow, avoidance of significant wear on the plasma gun electrode, a controlled method of quenching particles in the quench chamber, and the newly formed nanoparticles are cooled by a conduit. Mechanism to avoid sticking to the walls of the chamber, efficiency compared to ambient pressure, but constant but minimal system overpressure and / or recirculation of conditioned fluid used The continuous operation of a high throughput particle production system is provided.

Reduced Plasma Gun Faceplate Wear Long-term operation of a typical plasma-based nanoparticle production system can result in melting and distortion of the plasma gun faceplate, and a system shutdown can be required to replace it. While the plasma gun is operating, hot vaporized material and newly generated nanoparticles are exhausted into the quench chamber through the plasma gun outlet. As the particles pass through the plasma gun exit, significant heat is dissipated into the faceplate, which can melt and / or distort it. Since the proper shape of the faceplate is used to form or seal the cooling ring, distortion of the faceplate can lead to cooling fluid leakage. Since the cooling ring is used to control the temperature of the system, any melting or distortion of the faceplate can result in system shutdown and lost productivity.

  It has been found that increasing the diameter of the faceplate opening such that exposure of the faceplate to the hot plasma gun vapor outlet is minimized prevents melting and distortion of the faceplate. The cooling ring can then be sealed with a refractory material independent of the faceplate. The faceplate temperature is preferably below 900 ° C. during continuous operation of the plasma gun for more than 24 hours, more than 48 hours, more than 72 hours, more than 160 hours, more than 336 hours, more than 672 hours, or more than 1344 hours. , Kept below 450 ° C or below 100 ° C. 2E-F illustrate one embodiment of a modified plasma gun faceplate 230 and an independently sealed cooling ring 218. The modified plasma gun faceplate 230 is positioned so that the female electrode 204 can be held in place but not so close to the plasma gun outlet 212 that it is melted or distorted during continuous system operation. Independently, the sealed cooling ring 218 is sealed using a heat resistant plug 232. The heat resistant plug may be made from any heat resistant material, such as stainless steel, titanium, ceramic, or the like.

  This configuration of the high throughput particle production system results in the need to replace the plasma gun faceplate less frequently and allows continuous use of the high throughput particle production system. The system described is such that the particle production system is at least 6 hours, at least 12 hours, at least 24 hours, at least 48 hours, at least 72 hours (3 days), at least 336 hours (14 days), at least without faceplate replacement. Allows continuous operation at a flow rate of 672 hours (28 days), or at least 1344 hours (56 days), at least 9 grams / minute, at least 30 grams / minute, or at least 60 grams / minute.

Continuous Material Feeding System In a nanoparticle production system, input material, which can be in powder, pellet, rod, or other form, is fed through a material feed channel into a plasma gun near the plasma channel. . Material flowing into the plasma channel is evaporated by the plasma stream and discharged into the quench chamber. However, in most particle production systems that use a plasma gun, the heat of the plasma melts the powder particles that are fed into the plasma gun before reaching the plasma channel. It has been found that melted or partially melted raw material results in agglomeration of the raw material and clogging of the material delivery channel. As a result, the operation of the plasma gun must be stopped until it is cleaned, resulting in lost productivity and the inability to run the system continuously for extended periods of time.

  In high throughput systems, a constant flow of material is fed into the plasma channel and a continuous material feed system is used to allow continuous system operation and avoid interruption of the input raw material flow. The described system provides a device that automatically wipes out any raw material in the feed channel or allows the feed channel to be swept out while the continuous operation of the plasma gun continues. . In one embodiment, interruption of the input raw material flow into the plasma gun due to melting of the raw material in the feed channel is prevented by employing an alternating material injection port that is alternately cleaned or used in operation. Or it can be reduced. In addition or alternatively, a reciprocating plunger device is attached to the plasma gun to force the input raw material through the material injection port and into the plasma gun, avoiding significant raw material aggregation and clogging of the feed channel Can do. Additionally or alternatively, a pulsed air atomization system can be used to blow a sweep fluid into the material delivery system to clear material and prevent clogging of the channels.

  3A-C illustrate some embodiments of a continuous material delivery system. As illustrated in FIGS. 3A-C, the plasma gun 300 includes one or more material injection ports 314 configured to introduce raw materials into an internal chamber at a location within the plasma region 308. One or more material supply channels 316 can be provided in the female electrode 304 to connect the material source 318 to the material injection port 314. In some embodiments, a plurality of material injection ports 314 and material supply channels 316 are arranged in an annular configuration around the inner chamber. In some embodiments, a single material injection port 314 and a material supply channel 316 are used. In some embodiments, more than one material injection port 314 and material supply channel 316 are used. In some embodiments, the material injection port 314 and the material supply channel 316 are located closer to where the working gas is introduced into the inflow region 306 than where the plasma flow is formed. Configured to introduce raw materials into the internal chamber. In some embodiments, material injection port 314 and material supply channel 316 are configured to introduce raw material into the internal chamber at a location that is located closer to plasma gun outlet 312. The diameter of the material injection port 314 in the continuous material delivery system can range from about 1 millimeter to about 20 millimeters. The wider material injection port 314 is less clogged compared to the narrower material injection port. Preferably, the minimum diameter of the material injection port 314 is at least 3 millimeters to allow continuous material flow and continuous system operation.

  FIG. 3A illustrates one embodiment of a continuous material delivery system that uses alternating material injection ports. Such an embodiment includes two or more material injection ports 314 and a material supply channel 316. Disposed within each material supply channel 316 is a removable material supply tube 320 that connects the material source 318 to the material injection port 314. Optionally, the removable material supply tube 320 can be temporarily secured in place using a threaded connector or a latching mechanism. During operation of the high throughput particle production system, one or more material supply channels 316 can be active and one or more material supply channels 316 can be inactive. While the material supply channel 316 is inactive, the raw material does not flow through the material supply channel 316 and into the plasma gun. While the material supply channel 316 is active, the raw material flows from the material source 318, through the removable material supply tube 320 and the material supply channel 316, from the material injection port 314 and into the plasma gun. During long-term continuous use of a high-throughput particle production system, the radiant heat of the high temperature plasma can partially melt the raw material, causing the raw material to coagulate and the removable material supply tube 320 to become clogged. When it is detected that the removable material supply tube 320 is beginning to clog, the inactive material supply channel 316 may be activated and the active material supply channel 316 may be deactivated. While the material supply channel 316 is inactive, the removable material supply tube 320 may be removed from the material supply channel 316 to clear clogs, be cleaned, or replaced. The removable material supply tube 320 can then be re-fitted into the material supply channel 316 and activated as needed or otherwise desired. This switching of the activated state of the material supply channel 316 ensures that at least one material supply channel 316 remains active during operation of the high-throughput particle production system and allows continuous material feed flow. to be certain.

  FIG. 3B illustrates one embodiment of a continuous material delivery system that uses a reciprocating plunger device 322. The reciprocating plunger device 322 includes a plunger 324, a plunger housing 326, and a control mechanism. Plunger 324 is arranged to extend through material supply channel 316 when plunger 324 is in the extended position, as illustrated in FIG. 3B. Plunger 324 can also be retracted into plunger housing 326 as controlled by a control mechanism. The control mechanism may be any mechanism that allows the plunger 324 to reciprocate between an extended position and a retracted position. In some embodiments, the control mechanism may be a crankshaft or a hydraulic control system. In the embodiment illustrated in FIG. 3B, the control mechanism is a gas driven piston 328 that is activated by applying gas from the gas source 330 to the four-way direct acting solenoid valve 332. Direct acting spring return solenoid valve 332 alternately applies gas to the top and bottom of plunger housing 326 thereby activating piston 328 and allowing plunger 324 to reciprocate. In some embodiments, the gas used is argon. In some embodiments, the plunger reciprocates at a rate of at least 2 times / second, more preferably at least 6 times / second, or at least 8 times / second. In some embodiments, the plunger is ceramic to avoid attenuation and contamination due to the heat of the nearby plasma. In other embodiments, the plunger is made of or lined with tungsten.

  During operation of the particle production system, raw material is allowed to flow from the material source 318 across the plunger head 334 when the plunger 324 is in the retracted position. A reciprocating plunger control mechanism extends the plunger 324 through the material supply channel 316 end point and delivers powder to the internal chamber via the material injection port 314. Insertion of plunger 324 through material supply channel 316 alleviates clogging of material supply channel 316 and material injection port 314 caused by agglomeration of raw materials. Plunger 324 then reciprocates to the initial retracted position and restarts the cycle. In response to the reciprocation of the plunger 324 to its initial retracted position, the raw material can again flow from the material source 318 across the plunger head 334. Plunger 324 can repeat this movement at regular intervals to allow a constant flow of raw material into the interior chamber of plasma gun 300.

  FIG. 3C illustrates one embodiment of a continuous material delivery system that uses a pulsed gas spray system 334. In the pulsed gas spray system 334, the gas spray source 336 is disposed in a material supply channel 316 that is directed toward the infusion source port 314. The gas supply source 338 supplies a gas, preferably argon, to the gas spray source 336. The gas flow may be controlled by a two-way direct acting solenoid valve 340 to allow pulsed gas to be released from the gas spray source 336 into the material supply channel 316. A pressure regulator 342 and a pressure release valve 344 are disposed between the gas supply source 338 and the two-way direct acting solenoid valve 340 to adjust the pressure of the released gas. The high pressure pulsed gas can clear any agglomerated raw material in the material supply channel 316 and prevent clogging during operation of the high throughput particle production system.

  Providing a continuous material delivery system to the nanoparticle production system ensures that the system does not need to be shut down to clear the agglomerated raw material clogging the material supply channel. This allows a continuous flow of raw material into the high throughput particle production system, allowing long term system operation and throughput. The system described is such that the particle production system is at least 6 hours, at least 12 hours, at least 24 hours, at least 48 hours, at least 72 hours (3 days), at least 336 hours (14 days), at least 672 hours (28 days). , Or at least 1344 hours (56 days), allowing continuous operation at a raw material flow rate of at least 9 grams / minute, at least 30 grams / minute, or at least 60 grams / minute.

Reduced non-uniform wear of plasma gun electrodes The long-term operation of a typical plasma-based nanoparticle production system results in excessive pitting and erosion of the plasma gun electrode, necessitating a system shutdown to replace these worn parts I know that. While the plasma gun is in operation, working gas is introduced into the inflow region and continues to flow through the plasma channel formed between the male and female electrodes. The current applied to the working gas between the male and female electrodes excites the gas into the plasma stream, resulting in steady plasma arc formation between the electrodes. The uneven heat distribution caused by the steady plasma arc causes uneven wear on the plasma gun electrode. In particular, the electrodes are pitting during operation. Uneven electrode pitting and wear is caused by the working gas in the plasma region because some portion of the working gas is trapped within the electrode pitting or other wear and is thereby decelerated and cannot flow evenly through the plasma channel. Inconsistent flow of Inconsistent flow during particle formation is undesirable because it results in uncontrolled and uneven particle coalescence. Non-uniform pitting therefore leads to electrode replacement, resulting in system shutdown and lost productivity.

  It has been found that uneven wear of the plasma gun electrode can be avoided or slowed by applying a non-linear bulk flow direction of the working gas, preferably a substantial vortex spiral flow, across the electrode. The substantial vortex spiral flow of the working gas prevents a steady plasma arc by distributing the working gas evenly. This also prevents electrode pitting and the resulting interruption of system operation, allowing continuous use of high throughput particle production systems. In one embodiment, a working gas injection ring installed in the plasma gun prior to the plasma region can provide the necessary vortices. The working gas injection ring preferably contains one or more ports positioned annularly around the male electrode to generate an even gas flow distribution.

  3A, 3B, and 3C each illustrate a plasma gun 300 with a working gas injection ring 346. FIG. A working gas injection ring 346 is disposed in the channel formed by the male electrode 302 and the female electrode 304 and separates the inflow region 306 from the plenum chamber 348. The plenum chamber 348 preferably receives working gas from the gas inlet 310 and supplies working gas to the channel inlet region 306 through the inlet ring 364. The working gas is preferably supplied at a higher pressure in the plenum chamber 348 than in the inflow region 306 to avoid backflow through the working gas injection ring 346. In some embodiments, the injection ring 346 is ceramic. Preferably, the injection ring 346 includes one or more injection ports 350 through which working gas is supplied to the inflow region 306. In some embodiments, a plurality of injection ports 350 are disposed in an annular configuration around the male electrode 302 and are preferably spaced evenly. In one embodiment, the injection port 350 is configured to supply working gas to the inlet region 306 and ultimately to the plasma region 308 in a substantially spiral spiral pattern. In some embodiments, the injection port 350 is angled toward the male electrode 302 to induce a substantially spiral spiral pattern. In some embodiments, the injection port 350 is angled away from the male electrode 302 to induce a substantially spiral spiral pattern. The pressure in the plenum chamber 348 is higher than the pressure downstream of the plenum chamber 348 and the gas injection ring 346 to ensure that gas flows out of all nozzles. Due to the placement of the injection ring 346, the working gas is substantially vortexed in a spiral pattern, so that the plasma arc generated in the plasma region 308 is different on the male electrode 302 and the female electrode 304. , Thereby substantially avoiding pitting or uneven wear of male electrode 302 and female electrode 304.

  Electrode wear may also be reduced by utilizing a heat conductive metal to produce a male electrode 302 or a female electrode 304. Alternatively, all or part of male electrode 302 or female electrode 304 may be lined with a heat resistant conductive metal such as tungsten, niobium, molybdenum, tantalum, or rhenium. In some embodiments, the refractory conductive metal is tungsten. The male electrode 302 and the female electrode 304 need not be made of, or lined with, the same heat conductive material. In some embodiments, only the male electrode 302 is lined with a refractory conductive metal. In another embodiment, only the female electrode 304 is lined with a refractory conductive metal. In some embodiments, only the cylindrical channel 309 along the female electrode 304 is lined with a refractory conductive metal. Refractory conductive metals allow the electrodes to withstand the high temperatures produced by the plasma for longer periods of time, thereby comparing to the more frequently used conductive metals in plasma gun electrodes such as brass or copper. Reduce wear.

  This configuration of the high-throughput particle production system results in less frequent replacement of the plasma gun electrode, allowing continuous use of the high-throughput particle production system. The system described is such that the particle production system is at least 6 hours, at least 12 hours, at least 24 hours, at least 48 hours, at least 72 hours (3 days), at least 336 hours (14 days), at least without electrode replacement. Allows continuous operation at a flow rate of 672 hours (28 days), or at least 1344 hours (56 days), at least 9 grams / minute, at least 30 grams / minute, or at least 60 grams / minute.

Narrow particle size distribution through increased residence time Particle nucleation and surface growth occurs immediately after energy delivery and material evaporation in the cylindrical channel 309 of the plasma gun. The residence time during which the particles continue to solidify and coalesce continues to form a time after evaporation, until the particles are exhausted into the quench chamber and fully cooled. Longer residence times result in a narrower particle size distribution, which is desirable in the production of nanoparticles. Residence time can be increased by reducing the working gas flow rate through the plasma gun, but this results in an overall reduction in material throughput, which is undesirable in high throughput nanoparticle production systems.

  Widening the cylindrical channel 309 in the female electrode 304 sufficiently increases the residence time during particle formation without affecting the overall material throughput to produce nanoparticles with a narrow particle distribution I know you can. In some embodiments, the diameter of the cylindrical channel 309 is about 3 millimeters to about 20 millimeters. Preferably, the diameter of the cylindrical channel 309 is at least 4 millimeters. The average residence time of the particles in the plasma gun is at least 3 ms, at least 10 ms, or at least 40 ms.

  The described system is at least 6 hours, at least 12 hours, at least 24 hours, at least 48 hours, at least 72 hours (3 days), while the particle production system produces nanoparticles with a sufficiently narrow size distribution. Continuously operating at a flow rate of 336 hours (14 days), at least 672 hours (28 days), or at least 1344 hours (56 days), at least 9 grams / minute, at least 30 grams / minute, or at least 60 grams / minute Make it possible to do.

Super Turbulent Quench Chamber After exiting from the plasma gun into the quench chamber, the particles continue to grow due to solidification and coalescence of the material evaporated during the cooling process. This cooling process occurs in the quench chamber. In some cases, maintaining the reactive mixture at too high a temperature for too long can lead to over-agglomerated particles in the final product. An exemplary method for cooling newly formed nanoparticles involves mixing the high temperature reactive mixture and conditioned fluid in a frustoconical quenching chamber. The frustoconical shape of the quench chamber allows for increased turbulence of the conditioned fluid by redirecting the fluid flow, which further accelerates particle cooling. Additional turbulence may be provided by accelerating the rate of conditioned fluid provided to the quench chamber. The frustoconical shape of the quench chamber and the harmonic fluid flow rate provide some additional turbulence, but because of the smaller and better controlled nanoparticles produced by the high throughput system, A turbulent quench chamber is desirable. Some embodiments of super turbulent quench chambers are provided in US Patent Publication No. 2008/0277267, the contents of which are hereby incorporated by reference in their entirety.

  In a high throughput particle production system, turbulence-induced spray may be provided in the quench chamber to further increase turbulence and produce a super turbulent quench chamber. FIG. 4A illustrates one embodiment of a super turbulent quench chamber using turbulence induced spray. In response to exit of the reaction mixture from the plasma gun 402 through the plasma gun outlet 404, the reaction mixture flows into the quench chamber 406. As the hot reaction mixture moves into the quench chamber 406, it rapidly expands and begins to cool. Newly formed particles agglomerate and grow in size during the cooling process until the temperature of the material falls below the threshold temperature. The pressure gradient in quench chamber 406 causes particles to flow out of quench chamber 406 into cooling conduit 412 at quench chamber outlet 410. The pressure gradient may be provided by a suction force generator 408 located downstream of the quench chamber. The suction generator 408 may be, but is not limited to, a vacuum or a blower. As an alternative to or in addition to the suction generator 408, a pressure gradient may be provided by flowing the conditioned fluid into the quench chamber 406 at a higher pressure that flows out through the quench chamber outlet 410. Conditioned fluid can be provided to the gun box 414, which is fluidly connected to the quench chamber 406 by one or more ports 416.

  One or more turbulence inducing spray sources 420 inject turbulent fluid into quench chamber 406 to provide additional turbulence and accelerated cooling. In some embodiments, the turbulent fluid is the same type as the conditioned fluid. In some embodiments, the turbulent fluid is argon, but may also be a different inert gas. In some embodiments, the plurality of turbulence inducing spray sources 420 are arranged in an annular configuration around the plasma gun outlet 404. Preferably, in some embodiments using multiple turbulence inducing spray sources 420, the turbulence inducing spray sources 420 are uniformly spaced. In some embodiments where multiple turbulence induced spray sources 420 are employed, the turbulence induced spray source 420 may be independently supplied with turbulent fluid. In some embodiments, the turbulence inducing spray source 420 may be fluidly interconnected with a single turbulent fluid source. In some embodiments, the turbulence inducing spray source 420 is equipped with a tube 422 and a spray nozzle 424. However, in some embodiments, the spray nozzle 424 is not provided and turbulent fluid is discharged directly from the tube 422.

  Turbulent fluid can be supplied to the turbulence inducing spray source 420 at a pressure of 100-300 PSI to induce turbulence in the quench chamber. In some embodiments, the turbulent fluid is supplied at a pressure of 200 PSI. In some embodiments, the turbulent fluid is supplied at a pressure of 120 PSI. In some embodiments, the turbulent fluid is supplied at a pressure of 260 PSI. Preferably, the turbulence generated should have a Ray nozzle coefficient greater than 1000. The turbulence inducing spray source 420 is 20 relative to the flow of reactive reaction mixture through the plasma gun outlet 404 such that when the angle is greater than 90 degrees, the flow of conditioned fluid opposes the flow of reactive reaction mixture. The conditioned fluid can be emitted at ˜120 degrees. In some embodiments, the turbulence inducing spray source 420 can emit turbulent fluid perpendicular to the flow of the reactive reaction mixture through the plasma gun outlet 404, as illustrated in FIG. 4A. In embodiments with multiple turbulence induced spray sources 420, the turbulence induced spray source 420 prevents the turbulence induced spray source 420 from releasing turbulent fluid directly toward any other turbulence induced spray source 420. And may be angled away from the center of the annular form. In some embodiments, the turbulence inducing spray source 420 is angled 2-15 degrees away from the center of the annular form. In some embodiments, the turbulence inducing spray source 420 is angled 12 degrees away from the center of the annular form. In some embodiments, the turbulence inducing spray source 420 is angled 8 degrees away from the center of the annular form. In some embodiments, the turbulence inducing spray source 420 is angled 5 degrees away from the center of the annular form. In some embodiments, the turbulence inducing spray source 420 is angled 2 degrees away from the center of the annular form.

  The turbulence generated by the turbulence induced spray source 420 facilitates mixing of the conditioned fluid and the reaction mixture, thereby increasing the quench rate. The quench rate may be adjusted by modifying the amount of turbulence generated by the turbulence inducing spray source 420. For example, the turbulence induced spray may be angled either vertically by the material flow or by increasing the flow rate of the conditioned fluid released by the turbulence induced spray.

  An alternative embodiment that produces a turbulent flow increase in the super turbulent quench chamber 406 is illustrated in FIGS. 4B and 5. In this embodiment, turbulence inducing sprays are interconnected using ring structures 426 and 500. The ring structure 426 can be disposed in the quench chamber 406 such that a flow of reactive material exiting the plasma gun 402 through the plasma gun outlet 404 passes through the ring structure 426. Referring to FIG. 5, the ring structure 500 comprises an inner channel 502 that is fluidly connected to a turbulent fluid supply conduit 504 that can supply turbulent fluid to the ring structure. Inner channel 502 is configured to distribute turbulent fluid substantially evenly throughout ring structure 500. One or more outlet ports 506 are annularly disposed along the ring structure 500 to discharge turbulent fluid into the quench chamber. The outlet port 506 is 20-120 degrees relative to the flow of reactive reaction mixture through the plasma gun outlet 404 so that when the angle is greater than 90 degrees, the flow of turbulent fluid counteracts the flow of reactive reaction mixture. Can emit a turbulent fluid. In some embodiments, the outlet port 506 can emit turbulent fluid perpendicular to the flow of the reactive reaction mixture through the plasma gun outlet 404. In embodiments with multiple outlet ports 506, the outlet port 506 is spaced away from the center of the annular configuration so that the outlet port 506 does not release turbulent fluid directly toward any other outlet port 506. It may be angled. In some embodiments, the outlet port 506 is angled 2-15 degrees away from the center of the annular form. In some embodiments, the outlet port 506 is angled about 12 degrees away from the center of the annular form. In some embodiments, the outlet port 506 is angled about 8 degrees away from the center of the annular form. In some embodiments, the outlet port 506 is angled about 5 degrees away from the center of the annular form. In some embodiments, the outlet port 506 is angled about 2 degrees away from the center of the annular form.

  Turbulent fluid can be supplied to the outlet port 506 at a pressure of about 100-300 PSI to induce turbulence in the quench chamber. In some embodiments, the turbulent fluid is supplied at a pressure of about 200 PSI. In some embodiments, the turbulent fluid is supplied at a pressure of about 120 PSI. In some embodiments, the turbulent fluid is supplied at a pressure of about 260 PSI. Preferably, the turbulence generated should have a Ray nozzle coefficient greater than 1000.

  Super turbulent quenching chambers accelerate the cooling time of newly formed particles compared to more typical quenching chambers, resulting in smaller and more controlled particles. Super turbulent quenching chambers are desirable for high throughput particle production systems in order to continuously produce optimal and uniform size particles.

Laminar flow disruptor in a cooling conduit In a typical plasma-based particle production system, newly formed particles entrained in a conditioned fluid are passed from a quench chamber to a collector via a fluidly connected cooling conduit. To flow. In response to discharge from the quench chamber, the mixture of particles and conditioned fluid can be stabilized in a laminar flow while in a typical cooling conduit, even if there may be turbulence in the quench chamber. While in the cooling conduit, the particles are still warm and can agglomerate on the walls of the cooling conduit. After a certain cycle of operation of a typical particle production system, the accumulation of particles along the cooling conduit wall can lead to undesirable sized particles or clogging of the cooling conduit. Undesirable system shutdowns will therefore be required to manually clean the cooling conduit and return the system to proper function. A continuous high throughput plasma based particle production system preferably avoids particle accumulation in the cooling conduit.

  Accumulation of newly formed nanoparticles along the wall of the cooling conduit can be prevented or slowed down by providing a laminar flow disruptor in the cooling conduit. Laminar flow disrupters convert a laminar flow of a mixture into a non-laminar flow in a conditioned fluid and newly formed particles. Non-laminar flow redirects the particles and causes the entrained particles to collide with particles that adhere to the conduit wall. These collisions remove the deposited particles from the cooling conduit wall and allow the removed particles to re-enter the system stream. This prevents particle accumulation in the cooling conduit and eliminates the need for system shutdown due to particle accumulation in the cooling conduit. A laminar flow disruptor in the cooling conduit is therefore desirable for continuous operation of high throughput particle production systems with consistent material throughput.

  Several embodiments of laminar flow disruptors are illustrated in FIGS. 6A-D and 7. The combined conditioned fluid, turbulent fluid, and reaction mixture flow from quench chamber 602 through quench chamber exit port 604 and into cooling conduit 606. In some embodiments, a laminar flow disruptor 608 is present in the cooling conduit 606. The laminar flow disruptor 608 includes, but is not limited to, one or more blades, baffles, helical screws (FIG. 6A), ridges, bumps (FIG. 6B), air spray (FIG. 6C), rotary or steady axial An array of rods or blades (FIGS. 6D and 7), or other airflow redirecting devices may be included. Some embodiments may use more than one type of laminar flow disruptor. In some embodiments, the laminar flow disruptor 608 may move or rotate. In some embodiments, the laminar flow disruptor 608 is static.

  When the laminar flow disruptor 608 is a helical screw, as illustrated in FIG. 6A, the helical screw may extend through the entire length of the cooling conduit 606 or only a portion of the length of the cooling conduit. It may extend. Multiple helical thread sections may be used through the cooling conduit 606 when the helical screw extends only a portion of the length of the cooling conduit. Each section of the helical screw preferably makes at least one turn about the helical axis, however, some embodiments of the helical screw form of the laminar flow disruptor 608 need not be. As the conditioned fluid and particle mixture flows into the cooling conduit 606, the laminar flow is interrupted by being redirected by the helical screw to induce non-laminar flow.

  When the laminar flow disruptor 608 is one or more bumps, as illustrated in FIG. 6B, the bumps may be randomly distributed or evenly distributed through the cooling conduit. In some embodiments, the bumps may be more dense or concentrated in one section of the cooling conduit 606 than in another section. When the laminar flow disrupter 608 consists of a series of bumps, the bumps may be adjacent, but need not be.

  When the laminar flow disruptor 608 comprises one or more air spray sources, as illustrated in FIG. 6C, the laminar flow disruptor fluid source 610 is fluidly connected to the supply channel 612, which Laminar flow disturbing fluid can be injected into the cooling conduit 606 via the flow disturbing fluid injection port 614. Preferably, the laminar disturbing fluid is the same type of fluid as the conditioned fluid, but may be any other inert gas. If multiple air atomization sources are used, laminar turbulent fluid injection ports 614 may be annularly disposed at various points along the cooling conduit 606. In some embodiments, the laminar fluid injection port 614 is directed from the quench chamber 602. In some embodiments, the laminar fluid injection port 614 is oriented perpendicular to the wall of the cooling conduit 606 or in the direction of the quench chamber 602. When the high throughput particle production system is in operation, the force of the laminar turbulent fluid injected into the cooling conduit 606 alters the trajectory of the conditioned fluid and particle mixture in the cooling conduit 606, and A flow can be generated. This non-laminar flow prevents particles from accumulating along the walls of the cooling conduit 606.

  When the laminar flow disruptor is embodied by an axially arranged bar or blade, as illustrated in FIG. 6D, one or more laminar flow disruptors 608 may be used to mix the conditioned fluid and particles. It may be installed in the cooling conduit 606 to flow between the bars or blades. The blade or bar may rotate such that a substantially spiral vortex pattern can be generated when particles entrained by the conditioned fluid pass through the bar or blade. If multiple laminar flow disruptors 608 comprise rotating bars or blades, the bars or blades may rotate in the same direction or in different directions. If a blade is used, the blade may be in any orientation perpendicular to and parallel to the trajectory of the cooling conduit 606. FIG. 7 illustrates one embodiment of a laminar flow disruptor comprising a bar that rotates about an axis. In the present embodiment, the motor 702 is disposed at the center of the laminar flow disturber 700. Two or more bars 704 attached to the motor 702 are annularly arranged around the motor 702 and controlled thereby. During operation of the high throughput particle production system, the motor 702 rotates the bar 704 about the central axis. Optionally, stabilizing rim 706 may be positioned about the circumference of laminar flow disruptor 700 to limit the displacement of bar 702. The rotation of the bar 704 can cause rotation of the particles entrained in the conditioned fluid in the cooling conduit 606 and can generate a non-laminar flow. Non-laminar flow can cause removal of particles attached to the walls of the cooling conduit 606.

  Laminar flow disruptor 608 limits particle agglomeration along the wall of cooling conduit 606 by redirecting the material directed flow in cooling conduit 606. Some particles can still adhere to the conduit wall. However, constant flow redirection removes attached particles by causing the particles in the gas stream to collide with particles that adhere to the wall. The laminar flow disrupter results in continuous material flow by preventing clogging of the cooling conduit 606, shutting down the high throughput particle production system, and alleviating the need to clean the cooling conduit 606. A laminar flow disruptor in the cooling conduit of a high throughput particle production system is therefore desirable for continuous and consistent operation and material throughput.

  The described system is such that the particle production system is at least 6 hours, at least 12 hours, at least 24 hours, at least 48 hours, at least 72 hours (3 days), at least 336 hours (14 hours without clogging in the cooling conduit. Capable of continuously operating at a flow rate of at least 9 grams / minute, at least 30 grams / minute, or at least 60 grams / minute, at least 672 hours (28 days), or at least 1344 hours (56 days) To.

Gas delivery system with constant overpressure In a typical particle production system, the material throughput is generally maintained using a pressure gradient, allowing the particles to flow from the plasma gun to the collection device. The pressure gradient can be established by applying a suction force downstream of the collection device and generating a negative pressure for the upstream plasma gun and quench chamber. The particles are often collected in a collection device using a filter. However, during operation of a typical particle production system, the filter can clog, produce the desired pressure gradient, and require greater suction to ensure continuous particle throughput. When the filter is changed, the suction force needs to be reduced to produce the desired pressure gradient. However, suction forces can cause the internal pressure of the plasma gun or quench chamber to drop below ambient pressure, resulting in contamination due to the inflow of ambient gas during particle formation. Leakage can be mitigated by producing an overpressure in the gun box and quench chamber surrounding the plasma gun as compared to the ambient pressure. However, an overpressure that is too high results in excessive leakage from the system to the surrounding environment, and thus it is preferred that the overpressure be minimized. Providing a fixed overpressure in the system will not effectively minimize the pressure difference between system pressure and ambient pressure due to variations in suction force. For consistent throughput using high throughput particle production systems, the pressure differential between the system and the ambient environment is preferably minimized while maintaining a constant overpressure compared to the ambient pressure. The

  It has been found that a virtually constant system overpressure relative to ambient pressure can be maintained through the use of a gas supply system with a system overpressure module that is sensitive to ambient pressure. The system overpressure generated by the system overpressure module is configured to supply conditioned fluid to the gun box in a fixed amount above ambient pressure, thus minimizing system leakage and contamination. In some embodiments, the gas supply system delivers conditioned fluid to both the gun box and the collection system at a pressure that is minimally above ambient pressure but sufficient to maintain a pressure gradient. Alternatively, an independent gas supply system delivers conditioned fluid to the gun box and collection system. In another alternative, conditioned fluid is supplied only to the gun box and not to the collection device. The system allows a high throughput particle production system to remain constant within the gun box and quench chamber, but to maintain minimal system overpressure. Preferably, the system maintains an overpressure above at least one water column inch ambient pressure or at least two water columns inch ambient pressure. Preferably, the system maintains an overpressure greater than ambient pressure less than 10 inches of water, greater than ambient pressure less than 5 inches of water, or greater than ambient pressure less than 3 inches of water.

  FIG. 8 illustrates one embodiment of a gas delivery system 800 with constant overpressure. A pressure gradient is formed when conditioned fluid flows into the gun box 802 and suction is applied by a suction generator 804 downstream of the cooling conduit 806. In some embodiments, the suction generator 804 is a vacuum pump. In some embodiments, the suction generator 804 is a blower. In some embodiments, a suction generator is provided in collection device 808. Aspiration generator 804 draws used conditioned fluid through collection device 808, preferably through filter element 810. Filter element 810 is configured to remove residual particles in the conditioned fluid stream and produce a filtered output. During continuous operation of a high throughput particle production system, the filter element 810 can become clogged, resulting in the need to increase suction. System overpressure can be maintained by utilizing a system overpressure module 812 that supplies conditioned fluid to quench chamber 814 via gun box 802.

  In one embodiment of the gas delivery system 800, one or more conditioned fluid reservoirs 816 are integrated into the gas supply system and fluidly connected to the system overpressure module 812. In some embodiments, one or more conditioned fluid supply valves 818 may optionally be installed between any conditioned fluid reservoir 816 and the system overpressure module 812. In certain embodiments where more than one conditioned fluid reservoir 816 is used, the fluid types may be the same type or different types. In one embodiment, the conditioned fluid reservoir 816 contains argon. Conditioned fluid flows from the conditioned fluid reservoir 816 to the system overpressure module 812 via the conditioned fluid supply conduit 820.

  System overpressure module 812 regulates flow from conditioned fluid reservoir 816 to gun box 802. System overpressure module 812 ensures that conditioned fluid is supplied to gun box 802 with a constant but minimal overpressure relative to ambient pressure. In some embodiments, the system overpressure module 812 is contained within a single retractable unit. In some embodiments, the system overpressure module 812 is not contained within a single retractable unit. In some embodiments, the system overpressure module 812 is not stored in any unit, but may instead be a conduit, valve, and pressure regulator network. The system overpressure module 812 includes one or more pressure regulators 822, 824, and 826 that are fluidly coupled in a series configuration. In some embodiments, the system overpressure module 812 also includes one or more pressure release valves 828 and 830.

In one embodiment of the gas delivery system 800, conditioned fluid is transported to the system overpressure module 812 via a conditioned fluid supply conduit 820. The conditioned fluid reservoir 816 supplies conditioned fluid to the conditioned fluid supply conduit 820 and the system overpressure module 812 at the original pressure P ₁ (such as about 250-350 PSI). System overpressure module 812, the inlet pressure P _1, is set as compared to ambient pressure, it reduces the tempering fluid pressure to the outlet pressure P _4. In some embodiments, the outlet pressure P ₄ is above ambient pressure fixed amount. In some embodiments, the outlet pressure P ₄ has a fixed ratio as compared to the ambient pressure. In some embodiments, the system overpressure module 812 supplies conditioned fluid to the gun box 802 at an outlet pressure range that is approximately 1-12 inches of water above ambient pressure. In some embodiments, the system overpressure module 812 supplies conditioned fluid to the gun box 802 at an outlet pressure that is about 4 inches of water above ambient pressure. In some embodiments, the system overpressure module 812 supplies conditioned fluid to the gun box 802 at an outlet pressure that is about 8 inches of water above ambient pressure. In some embodiments, the system overpressure module 812 supplies conditioned fluid to the gun box 802 at an outlet pressure that is greater than about 2 inches of ambient pressure. In some embodiments, the system overpressure module 812 supplies conditioned fluid to the gun box 802 at an outlet pressure range that is approximately one inch of water above ambient pressure.

In some embodiments, each pressure regulator 822, 824, and 826 includes a control portion 832, 834, and 836 and a valve portion 838, 840, and 842. In some embodiments, at least one of the pressure regulators uses a diaphragm-based adjustment mechanism. Preferably, the diaphragm based adjustment mechanism comprises a diaphragm based demand valve. Typically, a first in-line pressure regulator 822 receives conditioned fluid from conditioned fluid supply conduit 820 at P ₁ . The control portion 838 uses the input from P ₁ and the ambient pressure to control the valve portion 832 and release conditioned fluid at the outlet pressure P ₂ (such as about 50 PSI above ambient pressure). In some embodiments, a pressure regulator 824 positioned in the second series, for receiving a tempering fluid at P _2. Control portion 840 uses the input pressure _{P 2} and the ambient pressure, to control the valve portion 834, to release the tempering fluid at outlet pressure _{P 3} (such as greater than about 2PSI ambient pressure). In some embodiments, a pressure regulator 826 positioned in the third series, for receiving a tempering fluid at P _3. Control portion 842 uses the input pressure P ₃ and the ambient pressure, to control the valve portion 836, to release the tempering fluid at outlet pressure P _4.

In some embodiments, the system overpressure module 812 optionally includes one or more independent pressure relief valves 828 and 830 that are fluidly coupled between the final pressure regulator 826 and the gun box 802. May be. In some embodiments, pressure release valves 828 and 830 are configured to vent gas to the surrounding environment when the received pressure is above the selected pressure. In some embodiments, the first pressure release valve 828 receives gas from the final series pressure regulator 826 at pressure P ₄ . In some embodiments, if P ₄ is above a selected threshold, the pressure release valve 828 vents gas to the surrounding environment and reduces the inlet pressure to the gun box 802. In some embodiments, the selected threshold is relatively high compared to ambient pressure so that, under normal operation, pressure release valve 828 is not activated. In some embodiments, the system overpressure module 812 includes a plurality of pressure release valves 828 and 830 having different sensitivities and set to different thresholds. Preferably, the second series pressure relief valve 830 has a lower threshold than the first series pressure relief valve 828.

  In high throughput particle production systems with continuous and consistent material throughput, it is desirable to avoid contamination by maintaining the pressure of the plasma gun and quench chamber to be above ambient pressure. Continuous operation by configuring the gas delivery system to deliver conditioned fluid to the gun box at a constant overpressure compared to the ambient pressure, while reducing the pressure differential between the system and the ambient environment Contamination of the resulting high throughput particle production system will be minimized. This allows for consistent material throughput and production of high quality nanoparticles.

Conditioned fluid purification and recirculation system A large amount of high purity conditioned fluid may be used to ensure a constant material flow through the nanoparticle production system. In a typical particle production system, spent conditioned fluid is generally vented into the surrounding environment. While this solution may be effective in producing smaller scale particles, venting of spent conditioned fluid into the surrounding environment is cost effective for high throughput particle production systems that are kept in continuous operation. Undesired or environmentally undesirable. Further, venting of spent conditioned fluid may slow or stop particle production due to frequent replacement of the conditioned fluid source tank. Recirculation of used conditioned fluid without purification results in particle production due to leakage into the system, raw material, or any secondary fluid (such as working gas or turbulent fluid) that is different from the conditioned fluid It will result in an accumulation of impurities that can be introduced into the system. Such impurities can include, but are not limited to, reactive oxidizing impurities, hydrogen gas, chloride compounds, or water. A cost effective high throughput particle production system recycles the conditioned fluid while maintaining the conditioned fluid purity. This results in less waste fluid, ensures higher quality particle production, and avoids a system shutdown that can occur when replacing an empty supply tank.

  The conditioned fluid can be recirculated in the high throughput particle production system to reduce costly conditioned fluid waste. It has been found that impurities can also be removed during recirculation of conditioned fluid using a conditioned fluid purification system, allowing a consistent pure conditioned fluid to be recirculated into the system. ing. The conditioned fluid purification and recirculation system provides continuous operation of the high throughput particle production system with recirculated and purified conditioned fluid and is cost effective for continuous operation of the high throughput particle production system. Solution can be provided.

  FIG. 9 illustrates one embodiment of a conditioned fluid purification and recirculation system in operation with a high throughput particle production system. While the high throughput particle production system is operating, working gas 902 and raw material 904 are introduced into plasma gun 906. The plasma gun 906 generates a plasma before it is exhausted into the quench chamber 908 to form a high temperature reactive mixture with the introduced raw materials and working gas. Once in the quench chamber 908, the hot reactive mixture is cooled by the conditioned fluid. Cooling particles entrained in the conditioned fluid stream pass through the cooling conduit 910 before being collected by the collection device 912. Spent conditioned fluid, along with any impurities, is drawn through the system by a suction generator 914, such as a vacuum or blower, before being introduced into the conditioned fluid purification system 916.

  The conditioned fluid purification system 916 may be any system configured to receive a used conditioned fluid and release a more purified conditioned fluid. FIG. 9 illustrates one embodiment of a conditioned fluid purification and recirculation system. In response to the flow of spent conditioned fluid into conditioned fluid purification system 916, compressor 918 forces spent conditioned fluid into gas purifier 920. The gas purifier 920 removes impurities from the gas, including but not limited to heating or ambient temperature getters, dryers, gravity separations, hydroxide-based dust collectors, or other chemical catalysts. The system may also be included. In some embodiments, removed gaseous impurities may be disposed in the ambient environment through the open vent 922. In some embodiments, impurities may be trapped on a replaceable cartridge.

  In some embodiments, a pressure release valve 924, a temperature control module 926, or a filter 928 may each optionally be disposed between the suction generator 914 and the compressor 918 and fluidly connected. The pressure release valve 924 may be configured to release spent conditioned fluid into the surroundings when the pressure exceeds a predetermined threshold. The temperature control module 926 is preferably a heat exchanger and may serve to reduce the temperature of the used conditioned fluid prior to purification. Filter 928 may be, but is not limited to, a particle filter or a chemical filter.

  One or more pressure regulators 930 may be positioned downstream of the gas purifier 920 before the purified conditioned fluid is directed to the gun box 934 to complete the recirculation cycle. The pressure regulator 930 may be configured to release the purified conditioned fluid at a predetermined outlet pressure. In some embodiments, the outlet pressure of the pressure regulator 930 is a fixed amount that exceeds the ambient pressure. In some embodiments, the outlet pressure of the pressure regulator 930 has a fixed ratio compared to the ambient pressure. In some embodiments, the pressure regulator 930 releases conditioned fluid in an outlet pressure range that is about 1-250 inches of water above ambient pressure. In some embodiments, such as when the conditioned fluid purification system 916 is configured to recirculate clarified conditioned fluid directly to the gun box 934, as illustrated in FIG. 930 may be configured to release purified conditioned fluid at an outlet pressure range that is about 1-12 inches of water above ambient pressure. In an alternative embodiment, such as when the conditioned fluid purification and recirculation system 916 is integrated into a system overpressure module (as described below and in FIG. 10), the pressure regulator 930 can adjust the ambient pressure. It may be configured to release the purified conditioned fluid in an outlet pressure range of about 12 to 250 inches of water. In some embodiments, one or more pressure release valves 932 may be disposed downstream of the pressure regulator 930 and prior to the gun box 934. If present, the pressure relief valve 932 can be configured to release the purified conditioned fluid at a predetermined pressure.

  In some embodiments, the conditioned fluid purification system 916 may include a back pressure flow loop 936 that can include one or more back pressure regulators 938. The back pressure flow loop diverts a portion of the purified conditioned fluid from the output of the gas purifier 920 to the main conduit of the system upstream of the compressor 918. In general, during operation of a high throughput particle production system, the back pressure flow loop 936 is inactive. However, pressure can sometimes increase within the system, and delivery of ultra high pressure to the gun box 934 can damage sensitive components of the high-throughput particle production system. The pressure can be relieved by venting the purified conditioned fluid into the surrounding environment. However, it is preferable to avoid waste of conditioned fluid. The conditioned fluid can be recovered by diverting a portion of the conditioned fluid upstream of the compressor, where the pressure is generally lower. Back pressure regulator 938 can be configured to activate back pressure flow loop 936 when the pressure exceeds a predetermined pressure.

  During operation of a high throughput particle production system, consistent throughput generally depends on a continuous flow of conditioned fluid that is nearly pure. Working gases and raw materials introduced during the particle production process also frequently introduce impurities and can degrade the quality of the produced nanoparticles if accumulated in the system. Disposal of spent conditioned fluid minimizes the accumulation of impurities, however, is not cost effective for high throughput particle production systems in continuous operation. A conditioned fluid purification and recirculation system can purify spent conditioned fluid and recirculate it through the system, enabling cost-effective continuous use of the high-throughput particle production system. Preferably, at least 50, at least 80 wt%, at least 90 wt%, or at least 99 wt% conditioned fluid introduced into the nanoparticle production system is purified and recycled.

Integration of a gas delivery system with constant overpressure and a conditioned fluid purification and recirculation system In a preferred embodiment of a high throughput particle production system, both a gas delivery system with constant overpressure and a conditioned fluid purification and recirculation system Is used. Since the output of the gas delivery system and the conditioned fluid purification and recirculation system can have different pressures, it is preferred that both systems be integrated prior to delivery of the conditioned fluid to the gun box. Through simultaneous use of both systems, the purified and recirculated conditioned fluid is provided to the gunbox with minimal pressure compared to ambient pressure to eliminate conditioned fluid, impurities, and system leaks that are discarded. Can be limited. In addition, the simultaneous use of the gas delivery system and the conditioned fluid purification and recirculation system ensures that sufficient conditioned fluid has a high throughput even if there is some loss of conditioned fluid during the particle production or recirculation process. Ensure that the system is supplied during continuous use of the particle production system.

  FIG. 10 illustrates one exemplary embodiment of a system overpressure module 1002 integrated with a conditioned fluid purification and recirculation system 1004. In this integrated system, a suction generator 1006, preferably a vacuum or blower, delivers used conditioned fluid to the conditioned fluid purification system 1004. In response to the spent conditioned fluid entering the fluid purification system 1004, the compressor 1008 urges the used conditioned fluid into the gas purifier 1010. In some embodiments, each of the pressure relief valve 1012, the temperature control module 1014, or the filter 1016 is optionally disposed between the suction generator 1006 and the compressor 1008 and may be fluidly connected thereto. Good.

The system overpressure module 1002 is configured to deliver conditioned fluid to the gun box 1018 at an outlet pressure P ₄ set relative to the ambient pressure. In some embodiments, the outlet pressure P ₄ is a fixed amount above the ambient pressure. In some embodiments, the outlet pressure P ₄ has a fixed ratio as compared to the ambient pressure. In some embodiments, the system overpressure module 1002 supplies conditioned fluid to the gun box 1018 at an outlet pressure range that is approximately 1-12 inches of water above ambient pressure. When system overpressure module 1002 is integrated with a conditioned fluid purification and recirculation system, system overpressure module 1002 receives conditioned fluid from more than one source. In some embodiments, the system overpressure module 1002, a pressure P _1, the tempering fluid from one or more tempering fluid reservoir 1020, at a pressure P _5, receiving from the temper fluid purification and recirculation system 1004 To do. In some embodiments, one or more conditioned fluid supply valves 1022 may optionally be installed between any conditioned fluid reservoir 1020 and the system overpressure module 1002.

In some embodiments, the system overpressure module 1002 includes one or more pressure regulators arranged in series along the conditioned fluid supply conduit 1024. As illustrated in FIG. 10, pressure regulators 1026, 1028, and 1030 include control portions 1032, 1034, and 1036 and valve portions 1038, 1040, and 1042, respectively. In some embodiments, at least one of the pressure regulators uses a diaphragm-based adjustment mechanism. Preferably, the diaphragm based adjustment mechanism comprises a diaphragm based demand valve. A first in-line pressure regulator 1026 receives conditioned fluid from one or more conditioned fluid reservoirs 1020 at an initial pressure P ₁ . The control portion 1032 uses the input from P ₁ and the ambient pressure to control the valve portion 1038 to release conditioned fluid at an outlet pressure P ₂ (such as about 50 PSI above ambient pressure). In some embodiments, a pressure regulator 1028 which is located in the second series, for receiving a tempering fluid at the input pressure P _2. Control portion 1034 uses the input pressure _{P 2} and the ambient pressure, to control the valve portion 1040, to release the tempering fluid at outlet pressure _{P 3} (such as greater than about 2PSI ambient pressure).

One or more pressure regulators 1044 may be disposed between the gas purifier 1010 and the system overpressure module 1002 downstream of the gas purifier 1010. The pressure regulator 1044 includes a control portion 1046 and a valve portion 1048. The pressure regulator 1044 may be configured to receive the purified conditioned fluid from the gas cleaner 1010 and release the purified conditioned fluid at a predetermined outlet pressure. The control portion 1046 uses the input from the input pressure and the ambient pressure to control the valve portion 1048 and release the conditioned fluid at the outlet pressure P ₅ (such as about 100 inches of water above ambient pressure). Optionally, the pressure relief valve 1050 is disposed downstream of the pressure regulator 1044, when P ₅ is above a predetermined threshold value, it may be configured to release the cleaned temper fluid into the surrounding.

The conditioned fluid purification system 1004 releases the purified conditioned fluid to the system overpressure module 1002 via the recirculation conduit 1052. Recirculation conduit 1052 connects to conditioned fluid supply conduit 1024 at junction 1054. FIG. 10 illustrates a joint 1054 disposed between a second pressure regulator 1028 arranged in series and a third pressure regulator 1030 arranged in series, the joint being tempered. It may be located at any location along the fluid supply conduit 1024. Preferably, P ₅ is at a pressure that is higher than the pressure in the conditioned fluid supply conduit 1024 immediately upstream of the junction 1054. For example, as illustrated in FIG. 10, P ₅ is preferably greater than P ₃ .

In the embodiment illustrated in FIG. 10, a third in-line pressure regulator 1030 in system overpressure module 1002 receives conditioned fluid at a pressure that depends on P ₃ and P ₅ . Control portion 1036 uses the input pressure and ambient pressure, to control the valve portion 1042, to release the tempering fluid at outlet pressure P _4.

  In some embodiments, the conditioned fluid purification system 1004 may include a back pressure flow loop 1056, which can include one or more back pressure regulators 1058. The back pressure flow loop diverts a portion of the conditioned fluid purified from the output of the gas purifier 1010 to the main conduit of the system upstream of the back compressor 1008. In general, during operation of the high throughput particle production system, the back pressure flow loop 1056 is inactive. Back pressure regulator 1058 can be configured to activate back pressure flow loop 1056 when the pressure exceeds a predetermined pressure.

In some embodiments, the system overpressure module 1002 includes one or more independent pressure release valves 1060 and 1062 that are optionally fluidly coupled between the final pressure regulator 1030 and the gun box 1018. May be. In some embodiments, pressure release valves 1060 and 1062 are configured to vent gas to the surrounding environment when the received pressure is above the selected pressure. In some embodiments, the first pressure relief valve 1060 receives gas at the pressure P ₄ from the final series pressure regulator 1030. In some embodiments, if P ₄ is above the selected threshold, the pressure release valve 1060 vents gas to the surrounding environment and reduces the inlet pressure to the gun box 1018. In some embodiments, the selected threshold is relatively high compared to ambient pressure so that pressure release valve 1060 is not activated under normal operation. In some embodiments, the system overpressure module 1002 includes a plurality of pressure release valves 1060 and 1062 having different sensitivities and set to different thresholds. Preferably, the second series pressure relief valve 1062 has a lower threshold than the first series pressure relief valve 1060.

  By being configured as described, the gas supply system and the conditioned fluid purification and recirculation system can be compared to the ambient pressure in the gun box, regardless of pressure fluctuations or ambient pressure fluctuations caused by the suction generator. Thus, it is integrated to supply a purified conditioned fluid at a constant overpressure. The high throughput particle production system in continuous use utilizes a substantial amount of conditioned fluid so that the conditioned fluid can be purified and recirculated at a pressure that is minimally above ambient pressure. It is preferable to have.

Filter Back Pulse In a typical particle production system, newly produced particles are collected in a collection device by flowing the system output through one or more filter elements. Particles entrained by the used conditioned fluid are retained by the filter element while the used conditioned fluid passes through the filter element and is evacuated or recirculated. However, during continuous operation of a high throughput particle production system, the filter element can become clogged with the accumulation of newly generated particles. System operation and material throughput can be maintained for a relatively short period of time by applying an increased suction force downstream of the collection device, but system shutdown eventually results in particle output. It is required to collect and clean and / or replace the filter element.

  A system shutdown due to a clogged clogging filter element can interrupt normal system operation and throughput by applying one or more back pulses to the filter, causing particles to be released and then collected in a collection vessel. Without being found, it can be minimized within a high throughput particle production system. Each back pulse may be generated using a burst of fluid, preferably a conditioned fluid. This burst can occur at relatively short intervals and high pressures compared to the operating pressure of the collection device. The pressure of each back pulse should be high enough to remove particles from the filter element and allow the particles to fall into the collection container. In some embodiments, the back pulse may invert the filter, but inversion of the filter element is not necessary for the present invention. The back pulse is applied manually, at regular intervals, or when the sensor detects a decrease in material flow rate or when the suction force required to maintain the desired flow rate increases beyond a predetermined threshold. May be. In some embodiments, the sensor may be a pressure sensor or a flow rate sensor. In some embodiments, a single back pulse may be used, while in other embodiments, the back pulse may occur in a series of two or more bursts.

  FIG. 11 illustrates one embodiment of a high throughput particle production system with a filter back pulse system. During particle production, newly generated particles flow from the plasma gun 1102 through the quench chamber 1104 and the cooling conduit 1106 and into the collection device 1108. Spent conditioned fluid passes through the filter element 1110 and newly produced particles may accumulate on the surface of the filter element 1110. In some embodiments, most or substantially all of the newly produced particles accumulate on the surface of the filter element 1110. Spent conditioned fluid may continue to be drawn from the collection device 1108 by the suction generator 1112, recirculated, vented to ambient pressure, or otherwise disposed. The suction force generator 1112 may be, for example, a vacuum or a blower. Once the particles begin to accumulate on the filter element 1110, the suction force can be continuously increased by the suction force generator 1112 to maintain a fixed material flow rate. Since the suction force generator 1112 cannot permanently increase the suction force and a consistent flow rate is desired, once the material flow rate falls below a predetermined threshold, for example, 95% of the desired material flow rate. %, Or, for example, below 90% of the desired material flow rate or, for example, below 80% of the desired material flow rate, or the suction generator 1112 When applying a suction force of 95% of volume, or for example, 90% of volume, or for example, greater than 80% of volume, the filter back pulse system operates to relieve pressure buildup and restore normal system operation May be. In some embodiments, a sensor 1114, such as a flow rate sensor or a pressure sensor, may be fixed to the suction generator 1112 and trigger the operation of the filter back pulse.

  In one embodiment of the filter backpulse system, a backpulse fluid reservoir 1116 is fluidly connected to the first pressure regulator 1118, which in turn is fluidly connected to the backpulse tank 1120. In some embodiments, the back pulse fluid reservoir 1116 contains a conditioned fluid, such as argon. The first pressure regulator 1118 backs the conditioned fluid at a predetermined pressure so that the back pulse tank 1120 is pressurized with the conditioned fluid at the predetermined pressure when the back pulse system is not operating. It is configured to discharge to the pulse tank 1120. In some embodiments, the first pressure regulator 1118 will release conditioned fluid to the back pulse tank 1120 at about 80 psi to about 140 psi. In some embodiments, the first pressure regulator 1118 will discharge conditioned fluid to the back pulse tank 1120 at about 100 psi to about 120 psi.

  In some embodiments, the back pulse tank 1120 is fluidly connected to the second pressure regulator 1122, which is connected to the back pulse discharge conduit 1124. The second pressure regulator is configured to release the conditioned fluid at a predetermined pressure. In some embodiments, the second pressure regulator 1122 is configured to release conditioned fluid at the same pressure that the first pressure regulator 1118 is configured to release conditioned fluid. . In other embodiments, the second pressure regulator 1122 is configured to release conditioned fluid at a lower pressure than the first pressure regulator 1118. Backpulse discharge conduit 1124 is arranged such that the conditioned fluid released by the backpulse system is directed toward filter element 1110 in a trajectory opposite to the used conditioned fluid flow during normal system operation. .

  In some embodiments, a two-way direct acting solenoid valve 1126 is disposed along the back pulse discharge conduit 1124. The two-way direct acting solenoid valve 1126 can act as a trigger mechanism for the filter back pulse system. In response to receiving a signal to engage the operation of the filter back pulse system, eg, a manual signal or a signal from sensor 1114, the two-way direct acting solenoid valve 1126 causes the conditioned fluid to be pressurized with a back pulse. From the tank 1120 can be discharged to the back pulse discharge conduit 1124 where it can be delivered to the filter element 1110. In some embodiments, the two-way direct acting solenoid valve 1126 releases a single pulse of conditioned fluid. In other embodiments, the two-way direct acting solenoid valve 1126 can emit a series of two or more pulses. The pulse length can be any length of time, but is typically about 0.1 seconds to about 0.5 seconds long. When the two-way direct acting solenoid valve 1126 emits a series of two or more pulses, there is typically a delay of about 0.1 seconds to about 0.5 seconds between the pulses.

  Once the back pulse system is minimized, particles that have accumulated on the surface of the filter element 1110 are removed. Typically, the removed particles can fall into the collection container 1128 and be retained. The clogged filter element 1110 can then continue to be used without requiring shutdown of the high throughput particle production system. The described system requires that the particle production system be at least 6 hours, at least 12 hours, at least 24 hours, at least 48 hours, at least 72 hours (3 days), without having to replace the filter element 1110 in the collection device 1108. Continuously operating at a flow rate of 336 hours (14 days), at least 672 hours (28 days), or at least 1344 hours (56 days), at least 9 grams / minute, at least 30 grams / minute, or at least 60 grams / minute Make it possible to do.

  The aforementioned features and preferences associated with “embodiments” are separate preferences and are not limited to only that particular embodiment. That is, they may be freely combined with features from other embodiments if technically feasible and may form a preferred combination of features.

  The description is presented to enable one skilled in the art to make and use the invention and is provided in the context of a patent application and its requirements. Various modifications to the described embodiments will be readily apparent to those skilled in the art, and the generic principles herein may be applied to other embodiments. Accordingly, the present invention is not intended to be limited to the embodiments shown, but is to be considered the broadest consistent with the principles and features described herein. Finally, the entire disclosures of the patents and publications referred to in this application are hereby incorporated by reference.

Claims (113)

A nanoparticle production system,
A plasma gun comprising a male electrode, a female electrode, and a working gas supply source, wherein the working gas supply source is formed between the male electrode and the female electrode A plasma gun configured to deliver a working gas in a spiral flow direction across the
A continuous feed system configured to feed material into the plasma gun at a rate of at least 9 grams / minute;
A quench chamber positioned after the plasma gun and including at least one reaction mixture input and at least one conditioned fluid input;
A cooling conduit configured to conduct nanoparticles entrained in a conditioned fluid stream from the quench chamber to a collector, the cooling conduit comprising a laminar flow disruptor;
A system overpressure module that maintains a pressure in the system above the measured ambient pressure;
A nanoparticle production system comprising a conditioned fluid purification and recirculation system.   The nanoparticle production system of claim 1, wherein the continuous delivery system comprises a reciprocating member for continuously sweeping a material delivery supply channel during operation of the nanoparticle production system.   The nanoparticle production system according to claim 2, wherein the reciprocating member reciprocates at a rate of at least 2 times / second.   The nanoparticle production system of claim 1, wherein the continuous delivery system comprises a pulsed gas spray for continuously sweeping a material delivery supply channel during operation of the nanoparticle production system.   The nanoparticle production system of claim 1, wherein the nanoproduction system is operable for at least 336 hours without replacement of the male or female electrode.   The nanoparticle production system of claim 1, wherein the quench chamber has a frustoconical shape and is configured to generate turbulent flow with a Ray nozzle coefficient greater than 1000 during operation.   The nanoparticle production system of claim 1, wherein the laminar flow disruptor comprises a blade, a baffle, a helical screw, a ridge, or a bump.   The nanoparticle production system of claim 1, wherein the particle production system is configured to operate continuously for at least 336 hours without clogging in the cooling conduit.   The nanoparticle production system of claim 1, wherein the pressure in the system is maintained at a pressure that is at least one inch of water above the measured ambient pressure.   The nanoparticle production system of claim 1, wherein at least 80% of the conditioned fluid introduced into the nanoparticle production system is purified and recycled. A nanoparticle production system,
A plasma gun comprising a male electrode, a female electrode, and a working gas supply source, wherein the working gas supply source is formed between the male electrode and the female electrode A plasma gun configured to deliver a working gas in a spiral flow direction across the
A continuous feed system configured to feed material into the plasma gun at a rate of at least 9 grams / minute;
A quench chamber positioned after the plasma gun and including at least one reaction mixture input and at least one conditioned fluid input;
A cooling conduit configured to conduct nanoparticles entrained in a conditioned fluid stream from the quench chamber to a collector, the cooling conduit comprising a laminar flow disruptor;
A system overpressure module that maintains a pressure in the system above the measured ambient pressure;
A particle collection device comprising a filter and a pump, wherein the pump draws the conditioned fluid through the filter during operation of the nanoparticle production system and the nanoparticles are on the surface of the filter A particle collection device configured to apply a suction force to the filter to be collected;
A backpulse system configured to apply one or more backpulses to the filter during operation of the nanoparticle production system to release nanoparticles collected on the surface of the filter;
A conditioned fluid purification and recirculation system.   The nanoparticle production system of claim 11, wherein the continuous delivery system comprises a reciprocating member for continuously sweeping a material delivery supply channel during operation of the nanoparticle production system.   13. The nanoparticle production system according to claim 12, wherein the reciprocating member reciprocates at a rate of at least 2 times / second.   12. The nanoparticle production system of claim 11, wherein the continuous delivery system comprises a pulsed gas spray for continuously sweeping a material delivery supply channel during operation of the nanoparticle production system.   12. The nanoparticle production system of claim 11, wherein the nanoproduction system is operable for at least 336 hours without replacement of the male or female electrode.   12. The nanoparticle production system of claim 11, wherein the quench chamber has a frustoconical shape and is configured to generate turbulent flow with a Ray nozzle coefficient greater than 1000 during operation.   The nanoparticle production system of claim 11, wherein the laminar flow disruptor comprises a blade, a baffle, a helical screw, a ridge, or a bump.   12. The nanoparticle production system of claim 11, wherein the particle production system is configured to operate continuously for at least 336 hours without clogging in the cooling conduit.   12. The nanoparticle production system of claim 11, wherein the pressure in the system is maintained at a pressure that is at least one inch of water above the measured ambient pressure.   12. The nanoparticle production system of claim 11, wherein at least 80% of the conditioned fluid introduced into the nanoparticle production system is purified and recirculated.   The nanoparticle production system according to claim 11, wherein the plasma gun includes a cooling ring arranged in an annular shape around the outlet of the plasma gun.   13. The nanoparticle production system according to claim 12, wherein the plasma gun includes a face plate, and the face plate is disposed on an outer surface of the plasma gun and joined to the cooling ring.   23. The nanoparticle production system of claim 22, wherein the face plate is maintained below 900 ° C. during continuous operation of the plasma gun for more than 160 hours.   12. The nanoparticle production system of claim 11, wherein the continuous feed system comprises a plurality of material injection ports having a minimum diameter of at least 1 mm.   The nanoparticle production system according to claim 11, wherein the male electrode or the female electrode is lined with tungsten.   12. The nanoparticle production system according to claim 11, wherein the average residence time of the particles in the plasma gun is at least 3 msec.   12. The back pulse system is configured to automatically apply one or more back pulses to the filter when a sensor detects a drop in a material flow below a predetermined threshold. Nanoparticle production system.   12. The back pulse system is configured to automatically apply one or more back pulses to the filter when a suction force through the filter increases above a predetermined threshold. Nanoparticle production system.   12. The nanoparticle production system of claim 11, wherein the back pulse system is configured to apply one or more back pulses with a pressure of 100 psi to 120 psi.   12. The nanoparticle production system of claim 11, wherein the back pulse system is configured to apply one or more back pulses comprising argon. A plasma gun useful for producing nanoparticles,
A male electrode and a female electrode, wherein either the male electrode or the female electrode is made of a conductive refractory metal; and
A working gas supply configured to deliver a working gas in a spiral flow direction across a plasma generation region formed between the male electrode and the female electrode;
And a face plate disposed on an outer surface of the plasma gun separated from a cooling ring.   32. The plasma gun of claim 31, wherein an average residence time of particles in the plasma gun is at least 3 msec.   32. The plasma gun according to claim 31, wherein the male electrode or the female electrode is lined with tungsten.   32. The plasma gun of claim 31, wherein the faceplate is maintained below 900 [deg.] C. during continuous operation of the plasma gun for more than 160 hours.   A nanoparticle production system comprising the plasma gun according to any one of claims 31 to 34. A nanoparticle production system,
With plasma gun,
A continuous feed system configured to feed material into the plasma gun at a rate of at least 9 grams / minute.   37. The nanoparticle production system of claim 36, wherein the continuous delivery system is configured to deliver material to the plasma gun for at least 336 hours without clogging.   37. The nanoparticle production system of claim 36, wherein the continuous feed system comprises a plurality of material feed supply channels for supplying raw materials to the plasma gun.   38. The nanoparticle production system of claim 36, wherein the continuous delivery system comprises a reciprocating member for continuously sweeping a material delivery supply channel during operation of the nanoparticle production system.   40. The nanoparticle production system of claim 39, wherein the reciprocating member reciprocates at a rate of at least 2 times / second.   38. The nanoparticle production system of claim 36, wherein the continuous delivery system comprises a pulsed gas spray for continuously sweeping a material delivery supply channel during operation of the nanoparticle production system.   37. The nanoparticle production system according to claim 36, wherein the plasma gun comprises a cooling ring arranged in an annular shape around the outlet of the plasma gun.   43. The nanoparticle production system of claim 42, wherein the plasma gun comprises a face plate, the face plate being disposed on an outer surface of the plasma gun and being joined to the cooling ring.   44. The nanoparticle production system of claim 43, wherein the faceplate is maintained below 900 ° C. during continuous operation of the plasma gun for more than 160 hours.   37. The nanoparticle production system of claim 36, wherein the plasma gun further comprises a plurality of material injection ports having a minimum diameter of at least 1 mm.   37. The nanoparticle production system according to claim 36, wherein the average residence time of particles in the plasma gun is at least 3 msec.   38. The nanoparticle production system of claim 36, further comprising a particle collection device positioned after the plasma gun and separating nanoparticles produced by the plasma gun from a conditioned fluid.   The particle production device comprises a filter and a pump, wherein the conditioned fluid is drawn through the filter and the nanoparticles are collected on the surface of the filter during operation of the nanoparticle production system. 48. The nanoparticle production system of claim 47, wherein the nanoparticle production system is configured to apply suction to the filter.   The particle production device further comprises a back pulse system, wherein the back pulse system applies one or more back pulses to the filter during operation of the nanoparticle production system and is collected on the surface of the filter. 49. The nanoparticle production system of claim 48, configured to release nanoparticles.   50. The back pulse system is configured to automatically apply one or more back pulses to the filter when a sensor detects a drop in the material flow below a predetermined threshold. Nanoparticle production system.   50. The back pulse system is configured to automatically apply one or more back pulses to the filter when a suction force through the filter increases above a predetermined threshold. Nanoparticle production system.   50. The nanoparticle production system of claim 49, wherein the back pulse system is configured to apply one or more back pulses with a pressure of 100 psi to 120 psi.   50. The nanoparticle production system of claim 49, wherein the back pulse system is configured to apply one or more back pulses comprising argon.   The plasma gun includes a male electrode, a female electrode, and a working gas supply source, and the working gas supply source is formed between the male electrode and the female electrode. 38. The nanoparticle production system of claim 36, wherein the nanoparticle production system is configured to deliver a working gas in a vortex spiral direction across.   55. The nanoparticle production system of claim 54, wherein the male or female electrode is lined with tungsten.   55. The nanoparticle production system of claim 54, wherein the working gas supply source comprises an injection ring, the injection ring being positioned in front of the plasma generation region and generating the vortex spiral direction.   57. The nanoparticle production system of claim 56, wherein the injection ring comprises a plurality of injection ports.   58. The nanoparticle production system according to claim 57, wherein the injection port is arranged in an annular shape around the male electrode.   59. The nanoparticle production system of claim 58, wherein the injection port is angled toward the male electrode.   59. The nanoparticle production system of claim 58, wherein the injection port is angled away from the male electrode.   55. The nanoparticle production system of claim 54, wherein the nanoproduction system is operable for at least 336 hours without replacement of the male or female electrode.   37. The nanoparticle production system of claim 36, further comprising a quench chamber positioned after the plasma gun and including at least one reaction mixture input and at least one conditioned fluid input.   64. The nanoparticle production system of claim 62, wherein the quench chamber has a frustoconical shape and is configured to generate turbulent flow with a Ray nozzle coefficient greater than 1000 during operation.   55. The nanoparticle production system of claim 54, further comprising a quench chamber positioned after the plasma gun and including at least one reaction mixture input and at least one conditioned fluid input.   65. The nanoparticle production system of claim 64, wherein the quench chamber has a frustoconical shape and is configured to generate turbulent flow with a Ray nozzle coefficient greater than 1000 during operation.   64. The nanoparticle production system of claim 62, further comprising a cooling conduit configured to conduct nanoparticles entrained in the conditioned fluid stream from the quench chamber to a collector.   68. The nanoparticle production system of claim 66, wherein the cooling conduit comprises a laminar flow disruptor.   68. The nanoparticle production system of claim 67, wherein the laminar flow disruptor comprises a blade, baffle, helical screw, ridge, or bump.   68. The nanoparticle production system of claim 67, wherein the particle production system is configured to operate continuously for at least 6 hours without clogging in the cooling conduit.   65. The nanoparticle production system of claim 64, further comprising a cooling conduit configured to conduct nanoparticles entrained in a conditioned fluid stream from the quench chamber to a collector.   72. The nanoparticle production system of claim 70, wherein the cooling conduit comprises a laminar flow disruptor.   72. The nanoparticle production system of claim 71, wherein the laminar flow disruptor comprises a blade, baffle, helical screw, ridge, or bump.   72. The nanoparticle production system of claim 71, wherein the particle production system is configured to operate continuously for at least 336 hours without clogging in the cooling conduit.   38. The nanoparticle production system of claim 36, further comprising a system overpressure module that maintains a pressure in the system above the measured ambient pressure.   75. The nanoparticle production system of claim 74, wherein the pressure in the system is maintained at a pressure that is at least one inch of water above the measured ambient pressure.   55. The nanoparticle production system of claim 54, further comprising a system overpressure module that maintains a pressure in the system above a measured ambient pressure.   64. The nanoparticle production system of claim 62, further comprising a system overpressure module that maintains a pressure in the system above a measured ambient pressure.   68. The nanoparticle production system of claim 67, further comprising a system overpressure module that maintains a pressure above the measured ambient pressure in the system.   77. The nanoparticle production system of claim 76, further comprising a conditioned fluid purification and recirculation system.   80. The nanoparticle production system of claim 79, wherein at least 80% of the conditioned fluid introduced into the nanoparticle production system is purified and recycled. A method of continuously feeding input material into a nanoparticle production system,
Feeding input material into the plasma gun through a first replaceable material supply tube;
After a reduced flow rate of the input material through the first replaceable material supply tube, feed the input material through the second replaceable material supply tube into the plasma gun;
Stopping the flow of input material through the first exchangeable material supply tube;
Reinitiating flow of input material through the first replaceable material supply tube into the plasma gun after cleaning or replacing the first replaceable material supply tube. A method of continuously feeding input material into a nanoparticle production system,
Feeding the input material into the plasma gun through the material feed supply channel;
Continuously sweeping the material delivery channel by forcing raw material into the plasma gun at a rate of at least 9 grams / minute.   82. The method of claim 81, wherein raw material is forced into the plasma gun by inserting a reciprocating member into the material delivery supply channel.   83. The method of claim 82, wherein the reciprocating member reciprocates at a rate of at least 2 times / second.   84. The method of claim 81, wherein raw material is forced into the plasma gun by pulsing gas into the material delivery supply channel. A nanoparticle production system,
With plasma gun,
A quench chamber positioned after the plasma gun and including at least one turbulent fluid input;
A cooling conduit configured to conduct nanoparticles entrained in the conditioned fluid stream from the quenching chamber to a collector; and
The cooling conduit comprises a laminar flow disruptor and the nanoparticle production system is configured to operate continuously for at least 6 hours without clogging.   87. The nanoparticle production system of claim 86, wherein the quench chamber has a frustoconical shape and is configured to generate turbulent flow with a Ray nozzle coefficient greater than 1000 during operation.   87. The nanoparticle production system of claim 86, wherein the laminar flow disruptor comprises a blade, baffle, helical screw, ridge, or bump.   90. The nanoparticle production system of claim 86, wherein the particle production system is configured to operate continuously for at least 336 hours without clogging in the cooling conduit.   87. The nanoparticle production system of claim 86, wherein the turbulent fluid input is arranged in a ring around the reaction mixture input.   94. The nanoparticle production system of claim 90, wherein the one or more turbulent fluid inputs are turbulence induced sprays.   92. The nanoparticle production system of claim 91, wherein the turbulence induced spray is directed toward a reaction mixture input.   92. The nanoparticle production system of claim 91, wherein the turbulence inducing spray is directed away from the reaction mixture input.   92. The nanoparticle production system of claim 91, wherein the turbulence inducing spray is directed perpendicular to the reaction mixture input.   94. The nanoparticle production system of claim 90, wherein the turbulent fluid input forms an interconnect ring. A nanoparticle production system,
With plasma gun,
A particle collection device comprising a filter and a pump, wherein the pump draws the conditioned fluid through the filter during operation of the nanoparticle production system and the nanoparticles are on the surface of the filter A particle collection device configured to apply a suction force to the filter to be collected;
A back pulse system configured to apply one or more back pulses to the filter during operation of the nanoparticle production system and to release the nanoparticles collected on the surface of the filter; system.   99. The back pulse system is configured to automatically apply one or more back pulses to the filter when a sensor detects a drop in a material flow that is below a predetermined threshold. Nanoparticle production system.   97. The back pulse system is configured to automatically apply one or more back pulses to the filter when a suction force through the filter increases above a predetermined threshold. Nanoparticle production system.   99. The nanoparticle production system of claim 96, wherein the back pulse system is configured to apply one or more back pulses with a pressure of 100 psi to 120 psi.   99. The nanoparticle production system of claim 96, wherein the back pulse system is configured to apply one or more back pulses comprising argon.   99. The nanoparticle production system of claim 96, wherein the nanoparticle production system is configured to operate for at least 6 hours without replacing the filter.   99. The nanoparticle production system of claim 96, further comprising a system overpressure module that maintains a pressure in the system above a measured ambient pressure.   105. The nanoparticle production system of claim 102, wherein the pressure in the system is maintained at a pressure that is at least one inch of water above the measured ambient pressure.   99. The nanoparticle production system of claim 96, further comprising a conditioned fluid purification and recirculation system.   105. The nanoparticle production system of claim 104, wherein at least 80% of the conditioned fluid introduced into the nanoparticle production system is purified and recycled. A nanoparticle production system,
With plasma gun,
A system overpressure module that maintains a pressure in the system above the measured ambient pressure;
A conditioned fluid purification and recirculation system;
A particle collection device comprising a filter and a pump, wherein the pump draws the conditioned fluid through the filter during operation of the nanoparticle production system and the nanoparticles are on the surface of the filter A particle collection device configured to apply a suction force to the filter to be collected;
A back pulse system configured to apply one or more back pulses to the filter during operation of the nanoparticle production system and to release the nanoparticles collected on the surface of the filter; system.   107. The back pulse system is configured to automatically apply one or more back pulses to the filter when a sensor detects a drop in a material flow that is below a predetermined threshold. Nanoparticle production system.   107. The back pulse system is configured to automatically apply one or more back pulses to the filter when a suction force through the filter increases above a predetermined threshold. Nanoparticle production system.   107. The nanoparticle production system of claim 106, wherein the back pulse system is configured to apply one or more back pulses with a pressure of 100 psi to 120 psi.   107. The nanoparticle production system of claim 106, wherein the back pulse system is configured to apply one or more back pulses comprising argon.   107. The nanoparticle production system of claim 106, wherein the nanoparticle production system is configured to operate for at least 6 hours without replacing the filter.   107. The nanoparticle production system of claim 106, wherein the pressure in the system is maintained at a pressure that is at least one inch of water above the measured ambient pressure.   107. The nanoparticle production system of claim 106, wherein at least 80% of the conditioned fluid introduced into the nanoparticle production system is purified and recycled.