This disclosure relates generally to pyrolysis tubes for material processing equipment (e.g., material deposition systems, etc.) and, more specifically, to pyrolysis tubes that are configured to improve the efficiency with which molecules of a precursor material are broken down, or “cracked,” into smaller reactive species. In addition, this disclosure relates to inserts for pyrolysis tubes, pyrolysis methods and equipment for depositing or otherwise processing materials, such as parylene.
Pyrolysis is a process by which an organic material is subjected, in an environment devoid of oxygen, to a temperature that is hot enough to decompose the organic material. More specifically, when an organic material is pyrolyzed, it undergoes an irreversible physical change. Among a wide variety of other uses, pyrolysis is used to crack unsubstituted and substituted [2.2] paracyclophanes, which are also commonly referred to as “Parylene dimers”—the precursors to various types of Parylene, or polyp-xylylene)—into reactive monomers.
Parylene dimers are typically pyrolyzed in a vacuum at temperatures that are sufficient to “crack” or break apart, molecules that are introduced into the pyrolysis tube. A pyrolysis temperature of about 680° C. is typical when depositing a parylene, or a polyp-xylylene). Pyrolysis of pure parylene dimers is typically considered to be a highly efficient process; however, since some contaminants are typically present in the parylene precursor, and possibly because pyrolysis tubes are rarely totally devoid of oxygen, the process of cracking parylene dimers can be inefficient, undesirably slow and result in byproducts that must be occasionally cleaned from the pyrolysis tube and other parts of the deposition equipment of which the pyrolysis tube is a part.
Because of the inefficiencies of the pyrolysis tubes of conventional material processing equipment (e.g., chemical vapor deposition (CVD) equipment, etc.) for depositing parylene, it typically takes several hours (e.g., three hours or longer) to deposit parylene to thicknesses of about 1 micrometer (μm) to about 18 μm or more.
This disclosure relates to pyrolysis tubes that are configured to efficiently crack parylene dimers and other materials, as well as to material processing equipment that includes such a pyrolysis tube, and to pyrolysis methods.
In one aspect, a pyrolysis tube according to this disclosure includes a primary conduit, which comprises a primary passage through the pyrolysis tube. The shape, dimensions and area of cross-sections taken transverse to the length of the primary passage may be uniform or substantially uniform (e.g., accounting for manufacturing tolerances, etc.) along the entire length of the pyrolysis tube. The primary passage is effectively subdivided into a plurality of sub-conduits, or channels. Accordingly, such a pyrolysis tube may be referred to as a “multi-channel pyrolysis tube.” In some embodiments, the longitudinal axes of the channels may be oriented parallel to one another, and parallel to the longitudinal axis of the primary passage, which may enable materials to flow directly through the lengths of the channels and, thus, through the primary passage of the pyrolysis tube. In other embodiments, the longitudinal axes of the channels may be configured to provide less direct flow paths. Without limitation, a channel may be curved, or even helical.
All of the channels may extend along the entire length of the primary conduit. Alternatively, one or more—even all—of the channels may extend only partially along the length of the primary conduit. Each channel may have a substantially uniform cross-sectional shape, substantially uniform dimensions and a substantially uniform area along its entire length.
The channels through a pyrolysis tube may be defined by one or more elongated elements that extend through at least a portion of the length of the pyrolysis tube. These elongated elements are referred to herein as “internal elements.” The internal elements may be embodied as one or more tubes that extend at least partially through the length of the primary passage of the pyrolysis tube. As another option, one or more of the internal elements of a pyrolysis tube may comprise a divider that extends across the primary conduit and at least partially along the length of the primary conduit or along the lengths of any other structures that may define channels through the primary conduit of the pyrolysis tube. In various embodiments, an internal element may be formed as an integral part of the pyrolysis tube, an internal element may be secured to one or more other internal elements and/or within (e.g., by welding, brazing, interference fit, etc.) the primary conduit through the pyrolysis tube or an internal element or an assembly of internal elements may comprise an insert that may be placed within and removed from the primary conduit of the pyrolysis tube.
The internal elements that define the channels within a pyrolysis tube according to this disclosure may be formed by a material that will withstand the conditions (e.g., the high temperatures, etc.) of pyrolysis. In some embodiments, the material from which the channel-defining elements of a pyrolysis tube are formed may comprise a thermally conductive material. Elements that are formed from a thermally conductive material may be continuous with, contact or otherwise convey heat from the outer wall of the pyrolysis tube, which defines the primary conduit through the pyrolysis tube, and improve the efficiency with which the heat is radiated throughout the interior of the pyrolysis tube.
A pyrolysis tube may be configured to distribute heat uniformly or substantially uniformly (i.e., within a certain range (e.g., twenty percent, ten percent, five percent, etc.) of the average temperature of the surfaces of the outer wall of the pyrolysis tube, etc.) throughout the interior of the pyrolysis tube.
A pyrolysis tube configured in accordance with teachings of this disclosure may enable pyrolysis to occur efficiently at a lower-than-conventional temperature (e.g., a temperature of less than 680° C., a temperature of 550° C. to 680° C., a temperature of less than 550° C., a temperature of less than 500° C., a temperature of about 400° C. to about 450° C., etc.). Such a configuration may also facilitate the use of smaller, or shorter, pyrolysis tubes. In addition, such a configuration may decrease the time required to effectively pyrolyze a parylene dimer and, thus, decrease the overall duration of time needed to deposit a parylene film of any desired thickness onto a substrate. By enabling the use of lower pyrolysis temperatures and increasing the efficiency with which parylene dimers are pyrolyzed, uniformity or substantially uniformity of the temperature across the primary passage through the pyrolysis tube may also decrease the frequency with which the pyrolysis tube or elements downstream from the pyrolysis tube are cleaned.
In another aspect, a material deposition system or another embodiment of material processing equipment may include a pyrolysis tube according to this disclosure. In some embodiments, the material processing equipment may comprise conventional material processing equipment with a conventionally configured pyrolysis tube. An insert for the pyrolysis tube may be configured to impart the pyrolysis tube with a plurality of channels. The insert may be configured to be introduced into and removed from a primary conduit of the conventionally configured pyrolysis tube. The use of an insert with a conventionally configured pyrolysis tube of conventional material processing equipment may improve the efficiency with which the pyrolysis tube pyrolyzes precursor material, enable the conventional material processing equipment to complete pyrolysis in a reduced duration of time and/or enable the conventional material processing equipment to operate at a reduced pyrolysis temperature.
In embodiments where the insert is configured to be removed from the pyrolysis tube, removability of the insert may enable inserts with a plurality of different configurations to be used with the same pyrolysis tube, as well as cleaning of the insert and/or the pyrolysis tube.
In other embodiments, material processing equipment may include a multi-channel pyrolysis tube with fixed internal elements.
Other aspects, as well as features and advantages of various aspects, of the disclosed subject matter will become apparent to those of ordinary skill in the art through consideration of the ensuing description, the accompanying drawings and the appended claims.
In the drawings:
With reference to
In use, the material deposition system 10 may be configured to receive a precursor material 50, convert the precursor material 50 to reactive species 55 and provide an environment in which molecules of the reactive species 55 may react with one another to form a polymer film 70 on one or more substrates 60. In the specific embodiment depicted by
In a variety of embodiments, including that depicted by
The embodiment of pyrolysis tube 30 shown in
In
Another embodiment of pyrolysis tube 30″′, which is depicted by
In some embodiments, such as that depicted by
The internal elements of a pyrolysis tube that incorporates teachings of this disclosure, as well as the shapes of the channels that are defined by the internal elements, may be configured to increase surface area within the pyrolysis tube and, thus, the likelihood that molecules of precursor material will collide with a surface or another molecule of precursor material within the pyrolysis tube. While the internal elements and the channels of a pyrolysis tube according to this disclosure may be configured to increase the surface area within the pyrolysis tube, they may also be configured not to interrupt or impede the flow of a precursor material and/or reactive species formed therefrom through the pyrolysis tube. As depicted by
The internal elements of a pyrolysis tube according to this disclosure (e.g., internal elements 34 (
Any suitable materials that will withstand the conditions of pyrolysis (e.g., temperatures of 400° C. or greater, temperatures of 500° C. or greater, temperatures of 600° C. or greater, temperatures of 700° C. or greater, temperatures of up to 800° C., etc.) may be used to form the internal elements of a pyrolysis tube or an insert according to this disclosure. A few non-limiting examples of suitable materials include steel, stainless steel, aluminum, an austenitic nickel-chromium-based super alloy, such as those available from Special Metals Corporation of New Hartford, N.Y., under the trademark INCONEL®, cobalt-chrome, titanium, silver and gold.
Experimentation revealed several indicators of the extent to which a pyrolysis tube 30 with a plurality of channels extending along at least a portion of its length improves the efficiency with which a precursor material 50 is cracked into reactive species 55. In the experiment, the performance of a pyrolysis tube 30 having the configuration shown in
Each pyrolysis tube was used to deposit a film of Parylene C onto a substrate under so-called “under-cracking” conditions, in which the precursor material (500 g of Parylene C dimer was used with each test of each pyrolysis tube) (i.e., Parylene C dimer) would be expected to condense at the entry point to the deposition chamber 40 (
A variety of results were analyzed. As shown by the graph of
In addition, observations of the entry point to the deposition chamber showed that little or no precursor material condensation was present when the multi-channel pyrolysis tube was used, while a significant amount of precursor material condensed at the entry point to the deposition chamber when the 30 inch conventional cylindrical pyrolysis tube was used. These results indicate that even when pyrolysis was conducted at a relatively low temperature, there was little or no under-cracking of the precursor material when the multi-channel pyrolysis tube was used. Thus, it appears that the multi-channel pyrolysis tube cracked molecules of the precursor material with greater efficiency than the conventionally configured pyrolysis tube. The improved cracking efficiency may reduce the frequency with which precursor material accumulates within the pyrolysis tube, which may reduce the frequency with which the pyrolysis tube should be cleaned, relative to the frequency with which conventionally configured pyrolysis tubes are cleaned.
Observations of the entry point to the deposition chamber also indicated that there may have been little or no over-cracking of the precursor material. Under the specific test parameters identified above, experimental results have shown that significant over-cracking, which includes the removal of chlorine (Cl) atoms from the Parylene C dimer, may result in a film that is green in color. No green color was present at the entry point to the deposition chamber.
These results support the belief that heat from radiation cannot completely crack molecules of precursor material by itself; an increased number of collisions between the molecules of precursor material increase the rate at which cracking occurs and, thus, the efficiency with which molecules of the precursor material are cracked. By separating the primary conduit through a pyrolysis tube into a plurality of channels, the rate at which collisions occur between molecules of precursor material is increased, which may lead to an increased rate of cracking, and to the increased efficiencies that were observed from the results of the above-described experimentation.
The results of the above-described experimentation also indicate that when a pyrolysis tube with a plurality of channels is used in a material deposition process, efficient and effective pyrolysis may occur at a relatively low temperature (e.g., 600° C., 575° C., 550° C., 500° C., 450° C., 425° C., etc., or less). They also suggest that, when higher (e.g., conventional, etc.) pyrolysis temperatures are used, the process of cracking molecules of a precursor material into reactive species may occur at a higher rate, which may also result in faster polymerization and deposition rates, and the deposition of a polymer film of a given thickness in a reduced amount of time.
As another option, by imparting a pyrolysis tube with a multi-channel configuration, its length may be shortened or effectively shortened (e.g., less of its length may be heated, etc.), which may reduce the size and cost of material deposition systems and/or the cost of operating material deposition systems (e.g., the energy required to heat the pyrolysis tube is decreased, etc.).
Although the foregoing disclosure provides many specifics, these should not be construed as limiting the scope of any of the appended claims, but merely as providing information pertinent to some specific embodiments that may fall within the scopes of the claims. Other embodiments may be devised which lie within the scopes of the claims. Features from different embodiments may be employed in any combination. All additions, deletions and modifications, as disclosed herein, that fall within the scopes of the claims are to be embraced by the claims.
This application is a division of U.S. patent application Ser. No. 14/457,690 filed on Jul. 30, 2015, titled MULTI-CHANNEL PYROLYSIS TUBES, MATERIAL DEPOSITION EQUIPMENT INCLUDING THE SAME AND ASSOCIATED METHODS (“the '690 application), which application claims the benefit of priority under 35 U.S.C. §119(e) to the Jan. 28, 2014 filing date of U.S. Provisional Patent Application No. 61/932,774, titled PYROLYSIS TUBE INCLUDING ONE OR MORE BAFFLES (“the '774 Provisional application”) is hereby made pursuant to. The entire disclosures of the '774 Provisional application and the '690 application are hereby incorporated herein.
Number | Date | Country | |
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61932774 | Jan 2014 | US |
Number | Date | Country | |
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Parent | 14457690 | Aug 2014 | US |
Child | 15217678 | US |