The present disclosure relates to three-dimensional (3D) micro-scale structures. More particularly, it relates to methods of making 3D micro-scale structures.
Three-dimensional (3D) micro/nanostructures with various shapes, architectures, and materials have recently been the subject of increased attention, because their dimensionality strongly influences their physical and chemical responses to surrounding environmental media as compared to two-dimensional (2D) micro/nanostructures. Conventional 3D fabrications are typically built using layer-by-layer (LBL) lithographic patterning methods, 3D printing, and/or self-aligned membrane projection lithography. More recently, origami-like, self-folding or self-assembly techniques have been developed.
Self-folding is a deterministic self-assembly process, providing a desirable strategy for creating three-dimensional (3D) micro-scale structures for 3D sensing, 3D metamaterials, drug delivery, cell cultures, cell encapsulation and micro-scale chemical container applications. In general terms, self-folding assembly entails the initial formation of a two-dimensional (2D) net of micro-scale panels connected to one another by a hinge material. The physical or chemical property of the hinge materials is caused to change, generating a surface tension force that causes the panels of the 2D net to self-fold relative to one another, resulting in a 3D micro-scale structure. In order to trigger or generate the physical or chemical property changes, external heat energy has been mainly used. For example, for thermal sensitive hinges, the phase transition (from solid to liquid) occurs when the hinge material absorbs heat energy, which generates surface tension forces for self-assembly. The heat energy is usually applied from an external source, such as a hotplate or a hot liquid bath, which requires direct contact between the heat source and the hinge materials. Another way to induce changes in the physical/chemical property is to apply environmental (e.g., pH or ionic strength) changes to solvent-sensitive hinge materials. Physical/chemical reactions occur when solvents are in contact with the hinge materials, triggering the self-assembly.
While viable, a drawback of conventional self-assembly processes is that the direct contact of heat energy sources or chemicals with the hinge materials critically limits its applications and reduces the manipulative capability of the self-assembly because the heat sources are not controllable and the environment around the microstructures is not accessible in many practical situations. For example, with many contemplated biomedical end use application, it is desirable to initiate the self-assembly process in a 2D net located within the human body (e.g., microrobots for surgery and tissue sampling, drug delivery); with these and other end use applications, direct contact heat source or chemical is not suitable. Moreover, direct heat energy sources, such as a hotplate or a hot liquid bath, usually have a high thermal mass, leading to a thermal lag (or time delay) from when the input energy is controlled to when the 2D net begin to self-fold or assemble. Thus, the assembling process cannot be precisely controlled using such methods.
The inventors of the present disclosure recognized that a need exists for 3D micro-scale structures and methods of making the same that overcome one or more of the above-mentioned problems.
Some aspects of the present disclosure relate to methods of manufacturing a 3D micro-scale structure. The method includes providing a 2D net. The 2D net includes a plurality of panels and a plurality of hinges. The panels (e.g., micro-scale panels) arranged in a pattern or array conducive to folding into a 3D shape. Each of the hinges interconnect immediately adjacent ones of the panels within the pattern. An energy source remote from the 2D net is powered to deliver energy to the 2D net. The delivered energy triggers the 2D net to self-fold into a 3D micro-scale structure. In this regard, the delivered energy creates an eddy current within at least one component of the 2D net, with the eddy current generating heat sufficient to melt the hinges. The melting hinges cause the corresponding panels associated with the melting hinges to fold or pivot relative to one another. In some embodiments, the energy source is a microwave energy source. In other embodiments, the energy source operates to deliver a magnetic field to the 2D net.
In some non-limiting embodiments, the 2D net incorporates at least one thin metal film (e.g., chromium) and polymeric hinges. The thin metal film absorbs electromagnetic microwaves and generates heat energy to induce reflow of the polymeric hinges, leading to self-assembly of 3D micro-scale structure. Since this assembly process does not require direct contact with a heat source or chemicals, micro-scale actuations can be achieved in a remote location without physical contact, resulting in the powerful capability to manipulate the 3D assembly process in situations where the heat sources and the environment around the microstructures are not controllable and accessible. Multiple folding configurations of the microstructures can also be achieved simultaneously with a single microwave energy source by forming different metal film thicknesses adjacent to the polymer hinges. Thus, remote-controlled self-assembly using microwave energy might be applied for the development of 3D micro-scale-sensors, micro-scale-microbots, and micro-scale-metamaterials.
In other non-limiting embodiments, the panels of the 2D include a metal (e.g., nickel), and the hinges are formed of a polymer with a relatively low melting point. A rapid changing magnetic field provided by an induction coil generates eddy current inside the panels, with heat dissipation of the eddy current being great enough to melt the polymeric hinges that in turn generate a surface tension force sufficient to articulate or fold the metallic panels relative to one another. The induction heating is localized to the metal panels, and is minimal, if any, effect on the surrounding environment. The induction magnetic field can penetrate through biomaterials. Induction heating can trigger self-assembly without harming live organs or tissues, and can be useful, for example, with biomedical applications such as cell encapsulation, cell culture, biomedical sensing, and drug delivery.
Aspects of the present disclosure are directed toward 3D micro-scale structures and methods of making the same, and in particular self-folding manufacturing techniques triggered by an indirect energy source. In general terms, the self-folding process is akin to origami in which a 2D micro-scale structure or net self-folds into a 3D micro-scale structure. For example,
As initially provided in the form of the 2D net 20, the panels 22 are arranged in an array conducive to folding into a 3D polyhedral shape, with facing edges of immediately adjacent ones of the panels 22 being connected to one another by a corresponding one of the hinges 24. Stated otherwise, in the 2D net array, various panels 22 are arranged side-by-side or edge-to-edge; one of the hinges 24 extends between and interconnects the corresponding edges thereof. For example, first and second panels 22a, 22b are identified in
In some embodiments, the 2D net 20 is configured such that when the 2D net 20 is subjected to energy from an indirect energy source, a temperature of the hinges 24 is raised to a critical point (e.g., melting point); the molten hinges 24 generate a surface tension force and cause the panels 22 to self-fold up into a 3D micro-scale structure (e.g., as a result of the polymer hinge melting (or reflow), a surface tension force is generated). For example,
The 2D net and resultant 3D micro-scale structures of the present disclosure can assume a wide variety of other shapes, such as any polyhedral shape, and are not limited to the cubic shape of
Against the above background and returning to
Microwave Energy Source
Some methods of the present disclosure use remote-controlled microwave energy with the ability to control the self-assembly process on a micro-scale. This process can also allow for the control of multiple folding angles of the panels 22 relative to one another simultaneously, even when using a single energy source for self-assembly, by adjusting the various thicknesses of the hinges 24, with each thickness responding differently to the microwave. The folding angles of each the panel of the panels 22 relative to one another in the resultant 3D micro-scale structure 40 are precisely controlled by tuning the power of the microwave sources in a remote location, resulting in a powerful manipulative capability of the 3D assembly process in situations where the heat sources and the environment around the microstructures are not controllable and accessible.
The microwave energy-based methods of the present disclosure are, in some embodiments, driven by Joule heating generated by eddy current within a transition body (e.g., thin metal film) provided with one or more or all of the hinges 24 and/or the joint structures 26. As a point of reference,
With the above in mind, a portion of a 2D net 60 in accordance with principles of the present disclosure is schematically shown in
With some methods of the present disclosure, the 2D net 60 is triggered to self-assemble to a 3D micro-scale structure by subjecting the 2D net 60 to microwave energy. For example, in
One example of a microwave energy source 80 useful with some methods of the present disclosure is shown in
Returning to
With the embodiment of
Magnetic Field Energy Source
Some methods of the present disclosure use a remote-controlled magnetic field energy source (electromagnetic waves), with the magnetic field producing localized heating as described below. The magnetic field can be biocompatible and safe to use around living tissues and organs, for example under circumstances where microwave energy may be harmful. The methods can be beneficial in situations where the heat sources and the environment around the microstructures are not controllable and accessible.
With reference to
With the above in mind, a portion of a 2D net 100 in accordance with principles of the present disclosure and useful with the magnetic field energy source or induction source methods of the present disclosure is schematically shown in
As shown in
With the magnetic field energy source-based methods of the present disclosure, the induced magnetic field can be biocompatible and safe to use around, for example, living tissues and organs. Since the heat is only generate on the surface of the metal material of the panels 102a-102d, the temperature increase during the self-assembly process is only limited at the micro-scale structure or 2D net 100, which minimizes the possibility of harm to the surrounding environment. Further, where the selected material for the hinges 106a-106c has a relatively low melting point (e.g., PCL with a melting point on the order of about 60° C.), the low melting point of the hinges 106a-106c promotes the self-assembly to occur at a relatively low temperature, furthering improving biocompatibility of the process. Thus, the induction driven remote-controlled self-assembly methods of the present disclosure can be suitable for various biomedical applications (e.g., self-assembly is triggered in situ by locating the 2D net 100 within a body of the patient, and operating an induction coil outside of the patient's body to generate a magnetic field that passes through the patient's skin, tissue, etc., and interact with the 2D net 100 as described above) such a cell encapsulation, culture and organization, smart drug delivery, etc.
Embodiments and advantages of features of the present disclosure are further illustrated by the following non-limiting examples, but the particular materials and amounts thereof recited in these examples, as well as other conditions and details, should not be construed to unduly limit the scope of the present disclosure.
Microwave Energy Source
Testing was performed to evaluate the microwave energy source-based methods of the present disclosure. With reference to
To quantitatively analyze the heat generation, inducing the hinge reflow by eddy current within the 20 nm thick Cr thin film, an infrared camera was used and recorded the surface temperature of the Cr thin film during the reflow process. The surface temperature of the 20 nm thick Cr thin film was found to rapidly and linearly increase from 28° C. (room temperature) to 177° C. in 15 seconds.
The heat generation within the Cr thin film under microwave radiation can be modeled by Faraday's law of induction and the definition of specific heat capacity. When an alternating magnetic field (B) is applied to a thin sheet of conductor (i.e., the 20 nm Cr film), a magnetic flux (ΦB=B×S, where S is the surface area of the conductor) is generated through the surface of the conductor. The time-varying magnetic flux is accompanied by an electric field (E, where ∇×E=−∂B/∂t), creating an eddy current (I), circulating in the Cr thin film against the resistance (R) of the thin metal film, which generates heat power (P) by Joule heating:
where P is the heat power generation per unit mass, Bp is the peak of magnetic field, d is the thickness of the conducting thin metal film, f is the frequency of the magnetic field, κ is a constant (κ=1 for thin sheet of conductor), ρ is the resistivity of the conducting thin metal film and D is the density of conducting thin metal film. From this model, when a constant P is generated, the temperature on the 20 nm Cr thin film was found to linearly increase with the increase of exposure time by ΔT=P·t/C, where ΔT is temperature changes, t is time, and C is specific heat capacity of the conducting material.
Provided as one illustrative example, to achieve 3D self-assembly of micro-scale structures using the heat generation from a nano-scale Cr thin film, a 20 nm thick Cr film was deposited on a 10×10 mm2 glass substrate. 2D micro-scale nets (having the pattern of
The folding angles of the 3D micro-scale structures of Example 1B (fabricated on a glass/Cr film substrate with a Cr film thickness of 20 nm) were captured at different exposure times. The folding of the cubic structure was found to start at about 6 seconds after microwave energy was applied, which reaches about 100° C. The structure was found to be totally folded to 90 degrees in 10 seconds. After the folding angle reached 90 degrees, even though microwave energy continued to be applied to the sample, the folding angle was found to remain at 90 degrees due to the interlocking between adjacent panels whose hinges have merged together.
To quantitatively analyze the assembly process, an equation of folding angles:
was derived from Equation (1) and ΔT=P·t/C, with an assumption that the folding angle is proportional to the heat generation P·t. In the equation, a is a constant of 2.7×10−18 and the parameter, β, indicates the initial time that starts folding.
To further evaluate the model of Equation (2), a glass/Cr film substrate with a Cr thickness of 10 nm and a glass/Cr film substrate with a Cr thickness of 15 nm were prepared, and the 2D nets of Example 1B were fabricated on each of the glass/Cr film substrates. The samples were exposed to microwave radiation at a frequency of 2.45 GHz, causing the 2D nets to self-fold. The folding angles of the structures during the self-folding process were captured at different exposure times.
A 2D micro-scale net akin to
Magnetic Field Energy Source
With the examples described below, various samples were energized by an indication system. The induction system included an induction coil made of copper wire with a diameter of 1 mm; the induction coil consisted of 8 turns of the copper wire, had a diameter of 1 cm, and a length of 1.5 cm. The induction coil was connected to a high frequency induction circuit that was powered by a power supply with a maximum power of around 200 W. The copper coil and induction circuit operated to generate a time-dependent magnetic field with a frequency of 5 MHz. A water-cooling system was also provided with the induction system, and operated to deliver water at a temperature of 10° C. to an environment of the induction coil. Unless otherwise noted, with each test, the sample in question was placed on top of piece of paper directly above the induction coil, and was centered relative to the induction coil.
Testing was performed to evaluate the magnetic field energy source-based methods of the present disclosure. To analyze the heat generation of a nickel thin film useful as a material of a panel of a 2D net (e.g., the panels 22 of the 2D net 20 of
To verify the reliability of the temperature measurements of Example 2A, simulations of the surface temperatures of Ni thin films under induction radiations were conducted using COMSOL Multiphysics. To simplify the simulation process, the Ni Sample Panel 1 was replaced with an Ni thin film plate with the sample total surface area in the simulator. The Ni plate was placed on a paper substrate above the induction coil. Actual coil temperatures were monitored during the assembly process and then applied to the coil in the simulator. It was found that the surface temperatures of the Ni plates increased from 18° C. to 58° C., which agrees well with the temperature measurements of Example 2A. The slight difference between the simulated and measured data may be due to the shape difference between the Ni Sample Panel 1 and the Ni plates, and the variations of induction frequency and power in the measured data.
To quantitatively analyze the temperatures on the surface of the Ni panels, additional sample panels were prepared as follows: Sample panels comprising a nickel thin film with dimensions of 500 μm×500 μm and a thickness of 5 μm (Ni Sample Panel 2) were prepared, and sample panels comprising nickel thin film with dimensions of 500 μm×500 μm and a thickness of 1 μm (Ni Sample Panel 3) were prepared. Each of Ni Sample Panels 1, 2 and 3 were placed on the induction coil of the induction system, and the induction system was operated to deliver an induction input power of 120 W for a 60 second test period during which the surface temperature of the Ni Sample Panel being tested was measured using an infrared camera.
Heat generation under the test conditions for Ni Sample Panels 1, 2, and 3 was also modeled using Equation (1). In the context of induction driven self-assembly, the terms of Equation (1) are: P is the eddy current power dissipation per unit mass, Bp is the magnetic field strength, d is the thickness of the conductor, f is the frequency of the magnetic field, κ is a constant (κ=1 for thin sheet of metal; κ=2 for a thin metal wire), ρ is the electrical resistance of the conductor, and D is the density of the conductor. The measured and modeled results for Example 2C are reported in
To further quantitatively analyze the temperatures on the surface of the Ni panels, additional sample panels were prepared as follows: Sample panels comprising a nickel thin film with dimensions of 200 μm×200 μm and a thickness of 15 μm (Ni Sample Panel 4) were prepared, and sample panels comprising nickel thin film with dimensions of 1000 μm×1000 μm and a thickness of 15 μm (Ni Sample Panel 5) were prepared. Each of Ni Sample Panels 1, 4 and 5 were placed on the induction coil of the induction system, and the induction system was operated to deliver an induction input power of 120 W for a 60 second test period during which the surface temperature of the Ni Sample Panel being tested was measured using an infrared camera. Heat generation under the test conditions for Ni Sample Panels 1, 4, and 5 was also modeled using Equation (1). The measured and modeled results for Example 2D are reported in
To further quantitatively analyze the temperatures on the surface of the Ni Panels, test panels of Ni Sample Panel 2 were subjected to differing induction powers. Each of the Ni Sample Panels 2 were placed on the induction coil of the induction system, and the induction system was operated to deliver an induction input power of 80 W (test 1), 120 W (test 2), or 200 W (test 3) for a 60 second test period during which the surface temperature of the Ni Sample Panel being tested was measured using an infrared camera. Heat generation under the conditions of test 1, test 2, and test 3 for Ni Sample Panel 2 was also modeled using Equation (1). The measured and modeled results for Example 2E are reported in
For all of the temperature experiments of Examples 2C-2E, the surface temperature of the Ni sample panel increases with an increase of induction radiation time, which can be explained by the heat generation equation W=P·t. Also, it can be observed from
A sample 2D net with the pattern of
The sample 2D net of Example 2F, supported by the paper substrate, was placed on the induction coil of the induction system. The induction system was operated to deliver an induction input power of 200 W, and the structure was monitored using a microscope and recorded using an optical camera.
As noted in
A sample 2D net with the pattern of
The results of Example 2G indicate that the induction magnetic field was able to penetrate through a biomaterial (beef tripe); self-assembly was triggered remotely without touching or seeing the sample to be assembled. Further, the heat generation was localized only at the 2D net and presented minimal potential harm to the biomaterial.
A sample 2D net with the pattern of
The results of Example 2H further indicates that the localized heat of induction-driven self-assembly limits the damage of heat to living tissues and organs. The induction-based self-assembly methods of the present disclosure are suitable for biomedical applications such as drug delivery systems, cell capture, cell encapsulation, etc.
The present disclosure provides a marked improvement over previous designs and techniques. Micro-scale 2D nets can be remotely or indirectly triggered to self-assemble into a 3D micro-scale structure, for example by causing localized heating sufficient to melt hinges of the 2D net. In some embodiments, microwave energy is utilized as a triggering source, generating an eddy current inside one or more components of the 2D net (e.g., a thin film metal) that in turn generate heat. In other embodiments, magnetic field energy is utilized as a triggering source, generating eddy current inside one or more components of the 2D net (e.g., a metal panel of the 2D net) that in turn generate heat. No physical contact is needed to trigger the folding process, which increases the manipulative ability of the self-assembly process. The self-assembly process can be easily and precisely controlled by tuning the reaction time of the microwave energy as well as the thickness of the conducting thin film. The remote-controlled self-assembly methods and corresponding structures of the present disclosure are suitable for diverse applications like microbots, 3D sensors, and 3D metamaterials, biomedical applications, etc.
Although the present disclosure has been described with reference to preferred embodiments, workers skilled in the art will recognize that changes can be made in form and detail without departing from the spirit and scope of the present disclosure.
This Non-Provisional Patent Application claims the benefit of the filing date of U.S. Provisional Patent Application Ser. No. 62/514,205, filed Jun. 2, 2017, the entire teachings of which are incorporated herein by reference.
This invention was made with government support under CMMI 1454293 awarded by the National Science Foundation. The government has certain rights in this invention.
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Number | Date | Country | |
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20190366492 A1 | Dec 2019 | US |
Number | Date | Country | |
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62514205 | Jun 2017 | US |