The disclosure relates to methods of demolding powder pressed ceramic structures having internal cavities such as channels and chambers and the like, and more particularly to apparatuses and processes for removing internal molds from green state powder-pressed ceramic structures having internal cavities while preserving the integrity of the powder-pressed structure.
Ceramics generally, and silicon carbide ceramic (SiC) in particular, can be desirable material for fluidic modules for flow chemistry production and/or laboratory work. Some ceramics, and SiC in particular, has relatively high thermal conductivity, useful in performing and controlling endothermic or exothermic reactions. Many ceramics have good physical durability and thermal shock resistance, and good chemical resistance. SiC in particular performs very well on these measures. But these properties, combined with high hardness and abrasiveness, make the practical production of fine or complex structures difficult, in particular the production of internal cavities such as channels or chambers and the like.
One of more of the present inventors and/or their colleagues have previously developed a powder pressing process for producing ceramic structures having internal cavities by pressing a binder-coated ceramic powder with a removeable mold—such as a mold formed of a relatively low temperature melting solid—positioned inside. After pressing, the mold is removed by heating, then the green state ceramic structure is debinded and sintered to form a final densified ceramic structure with the desired internal cavity(ies).
One or more of the present inventors has found that the previously developed powder pressing process can be dependent upon variations in in commercially available powder and binder mixtures. Some coater SiC powder products can work well, while in others, the pressed green state structure did not maintain structural integrity to the degree desirable during removal of the mold. Sometimes variations in performance may be present from batch to batch of the same powder product, not just from product to product. In an aspect of the problem, small cracks can be generated in the walls of the cavities of the powder pressed body during heating and removal of the mold material.
Recognizing the desirably to make the process independent of the quality of commercially available ceramic powder/binder mixtures, the present inventors have developed processes according to the present disclosure, according to which a method of removing an internal mold from within a green state powder pressed ceramic body includes applying energy to an internal mold the body to melt a material of the mold while applying a fluid pressure through a flexible membrane to at least two opposite external surfaces of the green state powder pressed ceramic body.
Also disclosed is an apparatus for removing an internal mold from within a green state powder pressed ceramic body includes an openable and closeable frame with an interior, one or more flexible membranes positioned within the frame having a first surface facing the interior and a second surface opposite the first forming at least part of an enclosed volume connected or to be connected to a supply of pressurized fluid, and a pathway through which a melted mold material can drain from the body.
By use of the method and/or the apparatus disclosed, a green state powder pressed ceramic body with internal cavities produced by an internal mold can be demolded by melting the material of the mold without producing or significantly producing interior surface cracks within the cavity.
Additional features and advantages will be set forth in the detailed description which follows, and will be readily apparent to those skilled in the art from that description or recognized by practicing the embodiments as described herein, including the detailed description which follows, the claims, as well as the appended drawings.
It is to be understood that both the foregoing general description and the following detailed description are merely exemplary, and are intended to provide an overview or framework to understanding the nature and character of the disclosure and the appended claims.
The accompanying drawings are included to provide a further understanding of principles of the disclosure, and are incorporated in, and constitute a part of, this specification. The drawings illustrate one or more embodiment(s) and, together with the description, serve to explain, by way of example, principles and operation of the disclosure. It is to be understood that various features of the disclosure disclosed in this specification and in the drawings can be used in any and all combinations. By way of non-limiting examples, the various features of the disclosure may be combined with one another according to the following embodiments.
The following is a description of the figures in the accompanying drawings. The figures are not necessarily to scale, and certain features and certain views of the figures may be shown exaggerated in scale or in schematic in the interest of clarity and conciseness.
In the drawings:
Additional features and advantages will be set forth in the detailed description which follows and will be apparent to those skilled in the art from the description, or recognized by practicing the embodiments as described in the following description, together with the claims and appended drawings.
As used herein, the term “and/or,” when used in a list of two or more items, means that any one of the listed items can be employed by itself, or any combination of two or more of the listed items can be employed. For example, if a composition is described as containing components A, B, and/or C, the composition can contain A alone; B alone; C alone; A and B in combination; A and C in combination; B and C in combination; or A, B, and C in combination.
In this document, relational terms, such as first and second, top and bottom, and the like, are used solely to distinguish one entity or action from another entity or action, without necessarily requiring or implying any actual such relationship or order between such entities or actions.
Modifications of the disclosure will occur to those skilled in the art and to those who make or use the disclosure. Therefore, it is understood that the embodiments shown in the drawings and described above are merely for illustrative purposes and not intended to limit the scope of the disclosure, which is defined by the following claims, as interpreted according to the principles of patent law, including the doctrine of equivalents.
For purposes of this disclosure, the term “coupled” (in all of its forms: couple, coupling, coupled, etc.) generally means the joining of two components directly or indirectly to one another. Such joining may be stationary in nature or movable in nature. Such joining may be achieved with the two components and any additional intermediate members being integrally formed as a single unitary body with one another or with the two components. Such joining may be permanent in nature, or may be removable or releasable in nature, unless otherwise stated.
As used herein, the term “about” means that amounts, sizes, formulations, parameters, and other quantities and characteristics are not and need not be exact, but may be approximate and/or larger or smaller, as desired, reflecting tolerances, conversion factors, rounding off, measurement error and the like, and other factors known to those of skill in the art. When the term “about” is used in describing a value or an end-point of a range, the disclosure should be understood to include the specific value or end-point referred to. Whether or not a numerical value or end-point of a range in the specification recites “about,” the numerical value or end-point of a range is intended to include two embodiments: one modified by “about,” and one not modified by “about.” It will be further understood that the end-points of each of the ranges are significant both in relation to the other end-point, and independently of the other end-point.
The terms “substantial,” “substantially,” and variations thereof as used herein are intended to note that a described feature is equal or approximately equal to a value or description. For example, a “substantially planar” surface is intended to denote a surface that is planar or approximately planar. Moreover, “substantially” is intended to denote that two values are equal or approximately equal. In some embodiments, “substantially” may denote values within about 10% of each other, such as within about 5% of each other, or within about 2% of each other.
Directional terms as used herein—for example up, down, right, left, front, back, top, bottom—are made only with reference to the figures as drawn and are not intended to imply absolute orientation.
As used herein the terms “the,” “a,” or “an,” mean “at least one,” and should not be limited to “only one” unless explicitly indicated to the contrary. Thus, for example, reference to “a component” includes embodiments having two or more such components unless the context clearly indicates otherwise.
As used herein, a “tortuous” passage refers to a passage having no line of sight directly through the passage and with the central path of the passage tracing more than one radius of curvature. Typical machining-based forming techniques are generally inadequate to form such a passage.
As used herein a “monolithic” ceramic or silicon carbide ceramic structure of course does not imply zero inhomogeneities in the ceramic structure at all scales. Monolithic, as the term is defined herein, refers to a ceramic or silicon carbide structure, with a internal cavities such as a tortuous passage extending therethrough, in which no inhomogeneities of the ceramic structure are present of sufficient size to extend from an external surface of the fluidic module to a surface of the tortuous passage.
With reference to
According to further aspects for silicon carbide embodiments, the body 200 of the fluidic module 300 has a density of at least 95% of a theoretical maximum density of silicon carbide, or even of at least 96, 97, 98, or 99% of theoretical maximum density.
According to further aspects of silicon carbide embodiments, the body 200 of the fluidic module 300 has an open porosity of less than 1%, or even of less than 0.5%, 0.4%, 0.2% or 0.1%.
According to still further aspects of embodiments, the body 200 of the module 300 has an internal pressure resistance under pressurized water testing of at least 50 Bar, or even at least 100 Bar, or 150 Bar.
The tortuous fluid passage P, according to embodiments, comprises a floor 212 and a ceiling 214 separated by a height h and two opposing sidewalls 216 joining the floor 212 and the ceiling 214. The sidewalls are separated by a width w (
According to embodiments, the interior surface 210 of the fluidic passage P where the sidewalls 216 meet the floor 212 has a radius of curvature (such as at location 218) of greater than or equal to 0.1 mm, or greater than or equal to 0.3, or even 0.6 mm.
With reference to
The process further can include the step of (partially) filling a press enclosure (or die) 100, the press enclosure 100 being closed with a plug 110, with binder-coated ceramic powder 120, as described in step 30 of
Next, the pressed body 150, now free from the press enclosure 100, is machined in selected locations, such as by drilling, to form holes or fluidic ports 160 extending from the outside of the pressed body 150 to the mold 130 (
Next, the pressed body 150 is demolded by being heated, preferably at a relatively high rate, such that the mold 130 is melted and removed from the pressed body 150 by flowing out of the pressed body 150, and/or by being blown and/or sucked out in addition. (
After the mold 130 has been melted and removed from the internal cavities or channels in the pressed body 150, the pressed body 150 is then fired (sintered) to densify and further solidify the pressed body into a monolithic silicon carbide body 200. (
As shown in the flowchart of
In alternative embodiments, the fluid source F may supplied gas under pressure such as compressed air or nitrogen, and the apparatus 400 can also include one or more flexible heating pads 272, 274, 276, 278 positioned on the first surface of the one or more flexible membranes 262, 264, 266, 268. A flexible heating pad of the apparatus can comprise (1) multiple zones in which input energy can be individually controlled and/or (2) multiple individually energizeable smaller heating pads, not shown, to which energy can be supplied by a source E of electrical energy.
In operation, in the apparatus of
According to additional aspects of the present invention, the flexible membrane through which pressure is applied may take the form of a fluid-tight bag enclosing the green state powder pressed ceramic body.
Process steps for one embodiment of demolding green pressed fluidic modules according to this aspect are shown in the flow chart of
Further in
The passage mold can be a wax-based material. As the green state powder pressed ceramic body 150 is heated by the warm fluid, the passage mold(s) 130 are also heated, and the mold material begins expanding, softening, and melting. The expansion produces an outward force on the interior walls of the passages within the body 150. The outward force is counteracted and/or balanced, at least in part, by the isostatic pressing force, represented by the arrows 330, applied to the exterior surface of the body 150 through the bag 320.
The melted mold material can move into ports such as ports IP1, IP2, IP, OP shown in
After the time period of step 516 is ended, the pressure inside the chamber 350 is reduced to atmospheric pressure in step 518, the chamber is opened and the bag 320 and body 150 are removed in step 522, and the bag 320 is removed from the body 150 in step 524. During steps 522 and 524, the body is preferably kept sufficiently warm (for example, at 50° C. or greater) to prevent re-solidification of the mold material, until any remaining mold material is completely removed by heating the body 150 in an oven (for example, at 175° C., in air), in step 526.
Prior to heating the body 150 in an oven in step 526, the body and the mold material may be in a state general depicted in the cross section of
According to another and alternative aspect of the present disclosure shown in the cross section of
The cross section of
In another additional or alternative aspect, as an alternative to the one or more ports or vents 386
In yet another additional or alternative aspect shown in the cross section of
In still another additional or alternative aspect shown in the cross section of
While exemplary embodiments and examples have been set forth for the purpose of illustration, the foregoing description is not intended in any way to limit the scope of disclosure and appended claims. Accordingly, variations and modifications may be made to the above-described embodiments and examples without departing substantially from the spirit and various principles of the disclosure. All such modifications and variations are intended to be included herein within the scope of this disclosure and protected by the following claims.
This application claims the benefit of priority under 35 U.S.C. § 119 of U.S. Provisional Application No. 63/065,079, filed Aug. 13, 2020, the disclosure of which is incorporated herein by reference in its entirety.
Filing Document | Filing Date | Country | Kind |
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PCT/US2021/038843 | 6/24/2021 | WO |
Number | Date | Country | |
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63065079 | Aug 2020 | US |