Patent Application
20110143930
The present invention relates to the field of the manufacture of nano-active materials. More particularly, the present invention relates to optimizing and customizing the size and concentration of a nano-active material on a substructure.
Nano-materials are quickly becoming commonplace in the scientific community as well as in commercial and industrial applications. Methods of conducting mechanical and chemical reactions oftentimes utilize nano-particles by themselves. However, other practices involve using a substructure to support a nano-scale component of a reaction. Oftentimes, nano-particles are impregnated into a substructure and the substructure processed, bonding the nano-particles to the walls of the substructure (i.e. calcination). One advantage to calcinating substructures containing nano-particles is that the particles will remain bonded to the substructure as fluid passes over it and reacts with the particles.
Many applications utilize catalysts to help in a reaction. In some applications, it is desirable to utilize small-scale catalysts on the order of nano-sized catalysts, such as nano-particles. Furthermore, it is also oftentimes desirable to use support structures to provide a substructure upon which the nano-particles reside. According to these processes, it is necessary to impregnate the substructure with the nano-sized catalysts.
Various methods of manufacturing nano-particles exist in the art. Methods of manufacturing nano-particles to be used as catalysts sometimes require the catalyst material itself and a carrier material upon which the catalyst is able to bond to when in a nano-sized state. Often times the practice of combining a catalyst and a carrier is accomplished by delivering the two materials to a combination chamber while the catalyst and the support are in a vapor or plasma state. The “clouds” of material are rapidly quenched and a combination material is provided in a solid nano-sized state. Next, a dispersion is created with the nano-sized combination material, a liquid and an adjunct additive causing mutual repulsion between near combination material particles. Next, this dispersion is impregnated into a support sub-structure. Finally a step of drying and calcination is performed to remove the liquid and bind the combination nano-particles to the substructure.
However, current methods of fabricating nano-particles on support substructures suffer from the lack of precision in controlling the size of the nano-active particles and the lack of a means for precise control over the total amount (or load) of nano-active material in a substructure. These deficiencies in the art lead to unsatisfactory or imprecise reactions and reaction rates.
The present invention discloses systems and methods of controlling the size of nano-particles on a support substructure. The present invention also discloses systems and methods of controlling the overall load of nano-particles within the substructure.
In some embodiments of the present invention, systems and methods are provided to control the size of a nano-active material on a carrier material, wherein the resulting particle is used in a catalytic process. This can be achieved by controlling the ratio of nano-active material and carrier material provided within a combination chamber.
In other embodiments of the present invention, systems and methods of performing multiple iterations of an impregnation step and a drying/calcination step are utilized to control the total amount of nano-active material with a substructure. According to these embodiments, the useful life of a substructure can be controlled.
In yet other embodiments of the present invention, the size of the nano-active particles is controlled and multiple iterations of the impregnation step are performed to control and ensure desired particle size and overall nano-active material loading within a substructure. According to these embodiments, the chemical selectivity and chemical activity of the loaded substructure can be precisely controlled.
Reference will now be made in detail to the embodiments of the methods and systems of manufacturing, examples of which are illustrated in the accompanying drawings. While the methods and systems will be described in conjunction with the embodiments below, it will be understood that they are not intended to limit the methods and systems of these embodiments and examples. On the contrary, the methods and systems are intended to cover alternatives, modifications and equivalents, which may be included within the spirit and scope of the methods and systems as defined by the appended claims. Furthermore, in the following detailed description, numerous specific details are set forth in order to more fully illustrate the methods and systems. However, it will be apparent to one of ordinary skill in the prior art that the methods and systems may be practiced without these specific details. In other instances, well-known methods and procedures, components and processes have not been described in detail so as not to unnecessarily obscure aspects of the optical detection module and recursive algorithm.
According to
In some embodiments of the present invention, the resulting nano-active material particles are less than 0.5 nm. In other embodiments, the resulting nano-active material particles range between 0.5 nm and 10 nm. In yet other embodiments, the resulting nano-active material particles are larger than 10 nm. For the purpose of this disclosure and the claimed invention, the term nano-sphere shall refer to any small scale particle that is at least partially spherically shaped with a size less than about 1000 nanometers.
Next, at step 130, the nano-scale spheres and a portion of adjuncts are added to a liquid, forming a liquid dispersion. The adjuncts are chosen for their ability to support mutual repulsion between adjacent nano-scale spheres. In some embodiments of the present invention, the adjuncts are an organic material.
At step 140, the liquid dispersion is used to impregnate a porous substructure. In some embodiments of the present invention, the substructure is a nano-scale substructure. In some embodiments of the present invention, the substructure is a ceramic substructure. In some embodiments of the present invention, the liquid dispersion is added to a container containing one or more porous substructures and allowed to impregnate the substructure naturally. In other embodiments of the present invention, the liquid dispersion is forced through one or more porous substructures. Next, at step 150 a drying/calcination step is performed to bond the nano-spheres to a surface within the porous substructure. The process ends at step 160.
It has been observed that the size of the nano-carrier material formed from cooling the vapor cloud is a function of system conditions, such as the time taken to cool the vapor cloud. However, the size of the nano-active material decorated upon the surface of the carrier material has been observed to be a function of the ratio of active material and carrier material vaporized. It has been observed that as the amount of pre-injection active material increases in relation to pre-injection carrier material, the particle size of the resulting post-cooling nano-active particle size increases. Likewise, as the amount of pre-injection active material decreases in relation to pre-injection carrier material, the particle size of the resulting post-cooling nano-active particle size decreases. This results from the probability of vaporized active material being found near other vaporized active material as the vapor is cooled and the vapor turns into particles. Accordingly, it is an object of the present invention to adjust the pre-injection ratio of active material to carrier material in order to tune the resulting size of the nano-active material decorated on the nano-carrier material.
At start step 200, active material and carrier material are provided at an initial ratio. At step 210, the active materials and the carrier materials are vaporized and injected into a processing chamber, forming a vapor cloud. At step 220, the vapor cloud is rapidly cooled, forming nano-scale spheres comprising nano-carrier particles decorated with nano-active material particles.
Next, at step 230, the nano-scale spheres are examined. In some embodiments of the present invention, a tunneling electron microscope is utilized to examine the nano-spheres, however it will become readily apparent to those having normal skill in the relevant art that a number of microscopy techniques, now present or later developed may be used to examine the nano-spheres. In other embodiments of the present invention, other means of examining the nano-spheres is utilized. For example, chemisorption techniques may be utilized to analyze the nano-spheres. Furthermore, other techniques of observing the nano-spheres will be readily apparent to those having ordinary skill in the art.
Next, at step 240, a choice is made whether to adjust the ratio of the starting material (i.e. the active-material and the carrier-material). The ratio of the starting materials are adjusted and injected into a chamber in a new ratio and are again vaporized at step 210, the vapor cooled at step 220 and the resulting nano-scale spheres are again examined. In some embodiments of the present invention, this process is repeated until the desired size nano-active material is found on the nano-carrier material of the nano-spheres. Once the desired size of the nano-active material is achieved, the adjustment step 240 is completed and the nano-scale spheres and a portion of adjuncts are added to a liquid at step 250, forming a liquid dispersion. At step 260, the liquid dispersion is used to impregnate a porous substructure. At step 270, a drying/calcination step is performed to bond the nano-spheres to a surface within the porous substructure. The process ends at step 280.
The resulting nano-spheres are able to be used in any variety of applications including, mechanical and chemical processes. In some embodiments of the present invention, the nano-active material is a catalyst. In some embodiments of the present invention, the nano-active material is nano-platinum and the substructure impregnated with nano-active platinum is utilized as a catalyst in oil refining applications.
In some embodiments of the present invention, a process of calibration is conducted to determine how the ratio of active material to carrier material affects the size of nano-active material on a nano-carrier material for any suitable combination of active material and carrier material.
At start step 201, active material and carrier material are provided. At step 211, a first occurrence of determining the relationship between the ratio of starting material and the size of nano-active particles begins. The number of iterations n is set to one, where n is an integer. Next, at step 221 the number m is determined, where m is equal to the number of different starting ratios to consider and record data from. Next, at step 231, a portion of active material in a vapor phase and a portion of carrier material in a vapor phase are combined in a nth ratio, forming a conglomerate vapor cloud. At step 241, the conglomerate vapor cloud is cooled, forming a nth sample of nano-spheres. At step 251, the nth sample of nano-spheres is examined and the size of the nano-active particles littered on the nano-carrier material is recorded. Next, at step 261, the number of different starting ratios, m, is considered and if that number is reached, the process ends at step 299. If the number m has not been reached, the integer n is increased by 1 at step 262 and the process repeats starting over at step 231. When the appropriate number of ratios have been considered, the process ends at step 299. When the process ends at step 299, the data is organized for later use.
After a process of calibration is done for a given set of starting materials, a process of manufacturing nano-spheres having a certain sized nano-active material may be accomplished without examining the nano-spheres, but rather by simply using the appropriate ratio of starting material as has been previously identified and recorded.
In the preferred embodiment, the size-tuned nano-particles are made to be used in chemical reactions. However, it is oftentimes the case that the nano-particles themselves, are not particularly useful in a chemical reaction because they will be quickly washed away when used with a liquid. Therefore, it is an object of the present invention to present the nano-particles in a useful form that can be used effectively in a chemical reaction. In some embodiments of the present invention, once size-tuned nano-particles are made, they are impregnated into a miniature substructure and bonded therein. In the preferred embodiment of the present invention, the substructure is an extrudate. For example, in oil refining and fine chemical reactions, an extrudate is the preferred means for exposing nano-active particles to the reaction.
Referring to
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In some embodiments of the present invention, an apparatus is disclosed for manufacturing nano-spheres and impregnating a substructure with the nano-spheres.
Once carrier material and active material is delivered to the vaporizer 405, it vaporizes the material and supplies the vaporized material to an injector gun 407. The injector gun 407 delivers vaporized material to a processing chamber 410. The vaporized material takes the form of a vapor cloud 412 within the processing chamber 410. Within the vapor cloud 412 is a concentration of vaporized active material and carrier material in some ratio.
In some embodiments of the present invention, a bleed line 418 is provided to evacuate the processing chamber 410. For example, it may be desirable to completely evacuate the processing chamber 410 after providing a first ratio of vaporized active material and vaporized carrier material before providing a second ratio of vaporized active material and vaporized carrier material.
The vapor cloud 412 is then cooled by cooling means 415. As the vapor cloud cools the vaporized active material and the vaporized active material bond together, forming nano-scale spheres 419 (indicated with a dot pattern) within supply means 420. The nano-scale spheres generally comprise a ball (not shown) of carrier material decorated with dots (not shown) of nano-active material. The size of the dots is dependent on the ratio of carrier material to active material supplied to the vaporizer 405.
In some embodiments of the present invention, the nano-scale spheres are examined by an examination instrument 430. According to these embodiments, a tunneling electron microscope is preferably used as the examination instrument 430, however it will become readily apparent to those having normal skill in the relevant art that a number of microscopy techniques, now present or later developed, may be used to examine the nano-spheres. In other embodiments of the present invention, chemisorption techniques can be utilized to analyze the nano-spheres. Furthermore, other techniques of observing the nano-spheres will be readily apparent to those having ordinary skill in the art.
In some embodiments of the present invention, the size of the nano-active material on the nano-spheres are examined. According to these embodiments, an operator is able to change the ratio of starting materials to tune the size of the nano-active materials. In some embodiments of the present invention, a controllable valve 435 is utilized to purge unwanted nano-spheres having nano-active material of an undesirable size and to allow size-tuned nano-particles through to be further processed. In some embodiments of the present invention, the controllable valve 435 is coupled to and controlled by the computer 425.
Once nano-spheres are produced having a desirable size, the nano-spheres are directed to a receptacle 440 and added to a liquid dispersion (indicated with a checkerboard pattern). In some embodiments of the present invention, a first chemistry tank 450 and a second chemistry tank 455 supply a liquid 451 and a portion of adjuncts 456, respectively, to the receptacle 440 to make up the liquid dispersion. The adjuncts 456 are chosen for their ability to support mutual repulsion between adjacent nano-scale spheres. In some embodiments of the present invention, the adjuncts 456 are an organic material.
The liquid dispersion is then directed to a chamber 460 and used to impregnate one or more substructures 465. A heating element 470 is provided for drying and calcination of the one or more substructures 465.
In some embodiments of the present invention, the computer 425 is coupled to the control module 404, the bleed line 418, the examination instrument 430, the controllable valve 435 and the heating element 470. According to these embodiments, the apparatus is fully automated based on instructions entered by an operator into the computer 425.
Once a new combination of active and carrier starting materials are chosen, it is desirable to calibrate the system in order to find how the ratio of starting material affects the size of the nano-active material decorated on the nano-carrier material. It is useful to be able to control the size of the nano-active material because the chemical activity of a nano-particle is oftentimes dependent on the size of the nano-particle. Therefore, depending upon the application and the size-dependent activity of the active material, one may desire a particular sized nano-active particle. As such, the particle size of the nano-active material is able to be adjusted to a particular size based on the calibration data according to some embodiments of the present invention. In some embodiments of the present invention, the particle size of the nano-active material is minimized. In some embodiments, the size of the nano-active material is minimized and multiple iterations of the impregnation step and the calcination step are performed to adjust the overall load of nano-active material within a substructure while maintaining the smallest possible scale (method discussed below).
As explained above, there are common mechanical and chemical applications which benefit from the use of nano-active materials. The size of the nano-active materials is important to these reactions because the chemical activity of the nano-active material changes with the size of the particles. It is also important to control the overall loading of a substructure in order to control the activity of chemical reactions. In general, the higher the overall loading of a substructure with nano-active material, the occurrence of the desired chemical reactions will take place at a greater rate as a desired chemistry is exposed to the to nano-active material located on the substructure (higher activity). One method of increasing activity is to increase the size of the nano-active material within the substructure because a larger surface area of active material will be exposed. However, as explained above, smaller particles of nano-active material are often needed to achieve the appropriate selectivity for a given application. Therefore, a method of increasing the overall loading (to increase activity) of a substructure while maintaining desired particle size (selectivity) is disclosed.
Next, at step 530, a choice is made whether to tune the size of the nano-active material decorated on the nano-spheres by adjusting the ratio of the starting materials (i.e. the carrier material and the active material). In the preferred embodiment of the present invention, the size of the nano-active particles is minimized. When the size of the nano-active material is tuned to the desired size, the nano-scale spheres and a portion of adjuncts are added to a liquid at step 540, forming a liquid dispersion. At step 550, the liquid dispersion is used to impregnate a porous substructure. At step 560, a drying/calcination step is performed to bond the nano-spheres to a surface within the porous substructure.
Next, at step 570, the impregnated substructures are examined to determine the overall loading of nano-spheres within and a decision is made whether to perform one or more impregnation iteration. As explained above, the size of the nano-active particles is minimized at step 530. According to this embodiment, the overall loading is able to be finely adjusted by performing one or more iterations of the impregnation step 550 and drying/calcination step 560 with the smallest common particle size. Subsequent iterations of impregnation increase the overall loading because the amount of space consumed by the nano-spheres within the substructure is very small compared to the total porous space available within the substructure. Once the size of the nano-active material is selected and the overall loading of the substructure is optimized, the process ends at step 580.
Oftentimes, a certain sized nano-active particle is desired based upon a given application due to the given reaction's chemical selectivity restraints. Furthermore, it is often desirable to increase the chemical activity of this reaction as well. In some embodiments of the present invention, a minimum sized nano-active material is manufactured on a nano-carrier material and a maximum amount of these resulting nano-spheres are impregnated into a support structure. As such, the effectiveness of the support structure and the active life of the substructure is maximized.
In some embodiments of the present invention, the active material is chosen for its propensity to serve as a catalyst and the carrier material is chosen for its propensity to bond to the active material. In some embodiments of the present invention, platinum is chosen as the catalyst and aluminum is chosen as a carrier material. In other embodiments, the carrier material is selected from among Al2O3, Si2O2, TiO2, C, AlSiO3, among other compounds. According to these embodiments, the size of the nano-active material is generally independently tunable regardless of the carrier material chosen.
The present invention has been described in terms of specific embodiments incorporating details to facilitate the understanding of principles of construction and operation of the invention. Such reference herein to specific embodiments and details thereof is not intended to limit the scope of the claims appended hereto. It will be readily apparent to one skilled in the art that other various modifications may be made and equivalents may be substituted for elements in the embodiments chosen for illustration without departing from the spirit and scope of the invention as defined by the claims.
This application claims priority to U.S. Provisional Patent Application Ser. No. 61/284,329, filed Dec. 15, 2009 and entitled “MATERIALS PROCESSING,” which is hereby incorporated herein by reference in its entirety as if set forth herein.
| Number | Date | Country | |
|---|---|---|---|
| 61284329 | Dec 2009 | US |
