This document relates to multi-surface nanoparticle deposition systems.
Nanoparticles have many applications, including applications in the field of medicine. There are various ways of creating nanoparticles.
In a first general aspect, a nanoparticle source includes a first end having an inlet configured to receive a flow of gas, a second end comprising an outlet through which nanoparticles exit the nanoparticle source, and two or more targets spaced apart and arranged about an axis extending from the first end to the second end. At least one of the targets is hollow, and the inlet is arranged to direct a flow of the gas through the hollow target, between at least two of the targets, or both. The gas impacts the targets, releasing atoms from the target and through the second end of the nanoparticle source. The targets may be arranged lengthwise from the first end to the second end of the nanoparticle source, and may be arranged concentrically about the axis.
Implementations may include one or more of the following features.
In some cases, the aspect ratio of at least one of the targets is 1:1 or less (e.g., 1:2 or less, 1:4 or less, 1:6 or less, 1:8 or less, 1:10 or less, or 1:16 or less. In certain cases, the aspect ratio is 1:32 or greater. In some examples, the aspect ratio of at least one of the targets is in a range between 1:1 and 1:32 inclusive, in a range between 1:2 and 1:16 inclusive, in a range between 1:4 and 1:10 inclusive, or in a range between 1:6 and 1:8 inclusive.
In certain cases, the nanoparticle source includes a magnet proximate the second end of the nanoparticle source. The magnet is arranged to provide a magnetic field that controls movement of the gas through the nanoparticle source. The magnet may be coupled to an end of one of the targets. In some cases, the magnet forms an extension of the target to which it is coupled. The magnet may be a circular magnet having the same shape (e.g., same inner diameter and outer diameter) as the target to which the magnet is coupled. In certain cases, the magnet is a circular magnet, and an inner diameter of the circular magnet is greater than or equal to the outer diameter of the target to which the circular magnet is coupled. The magnet may include materials such as, for example, samarium cobalt, neodymium cobalt, or a combination thereof.
The targets may be arranged concentrically about the axis. In some cases, the targets define an opening between the targets, and the inlet is arranged to deliver a flow of gas through the opening and toward the second end of the nanoparticle source. In certain cases, one of the targets is a cylinder centered lengthwise about the axis. One or more of the targets may be tube targets. The targets may include a single target material or two or more target materials. In some cases, at least two of the targets include different target materials. In certain cases, at least one of the targets includes segments of two or more different target materials. The target materials may include, for example, Au, Ag, Fe, FeCo, Gd, SiO2, Si, C, N, Al, Mg, or a combination thereof.
Some implementations include a cooling block, and at least some of the targets may be positioned in openings defined by the cooling block. The cooling block may be, for example, rectangular, cylindrical, or tubular. A surface of the cooling block (e.g., an inner surface or an outer surface of a tubular cooling block) may form a target. The target may include, for example, Au, Fe, Co, Ni, Si, Ti, N, Mg, C, or any combination thereof. In some cases, the cooling block defines a cooling chamber configured to receive a cooling fluid. The cooling block defines openings, and targets are positioned in the openings defined in the cooling block. The openings may form an array or one or more rings in the cooling block. The targets may be tube targets. The targets may be positioned in the openings defined by the cooling block and arranged in an array or in one or more concentric rings about the axis.
A nanoparticle source may include two or more cooling blocks. Each cooling block may be independently cooled. When the cooling block is rectangular, the nanoparticle source may include one or more additional rectangular cooling blocks and additional targets, wherein each additional rectangular cooling block defines additional openings, and the additional targets are positioned in the additional openings. Each additional rectangular cooling block may be positioned adjacent at least one other rectangular cooling block. When the cooling block is cylindrical or tubular, the nanoparticle source may include one or more additional tubular cooling blocks and additional tube targets, and each additional tubular cooling block may be arranged concentrically about a central cylindrical or tubular cooling block. Each additional tubular cooling block may define additional openings, and additional tube targets may be positioned in the additional openings and arranged (e.g., in one or more concentric rings) about the axis.
In some cases, the nanoparticle source includes a coil positioned about the nanoparticle source. The coil includes a current inlet and a current outlet and is configured to generate a magnetic field in each of the targets.
A second general aspect includes nanoparticles formed by any one of the nanoparticle sources described herein. In some cases, the nanoparticles are homogenous. In certain cases, the nanoparticles include a core and a shell. The core and the shell may include different materials, such as Fe, FeCo, Au, SiO2, Fe5Si3, Fe3Si, Fe16N2, FeN, or a combination thereof.
A third general aspect includes use of any one of the nanoparticle sources described herein to form nanoparticles.
A fourth general aspect includes forming nanoparticles by introducing a sputtering gas into any of the nanoparticle sources described herein via the inlet, ionizing the gas, and passing the ionized gas through a plasma region in the opening(s) between adjacent targets or through the targets to liberate atoms from the target, thereby yielding a gas comprising the liberated atoms. The gas including the liberated atoms is condensed to yield nanoparticles.
Implementations can provide any or all of the following advantages. Creation of nanoparticles can be improved. Nanoparticles of heterogeneous structure can be generated more efficiently and on a larger scale.
The details of one or more implementations are set forth in the accompanying drawings and the description below. Other features and advantages will be apparent from the description and drawings, and from the claims.
This document describes multi-surface nanoparticle sources and deposition systems and methods that are scalable for mass production. As described herein, a multi-surface nanoparticle source has two or more internal targets, so that the nanoparticle source has multiple surfaces. At least one of the targets is hollow. As used herein, a “hollow” target generally refers to a target having a lengthwise opening, such that a gas provided to a first end of the target flows lengthwise through the target and out a second end of the target. A “tube” target generally refers to a cylindrical target having a lengthwise opening, such that gas provided to a first end of the tube target flows lengthwise through the tube target and out a second end of the tube target.
A multi-surface nanoparticle source includes a first end having an inlet configured to receive a flow of gas, a second end comprising an outlet through which nanoparticles exit the multi-surface nanoparticle source, and two or more targets spaced apart and arranged about an axis extending from the first end to the second end of the multi-surface nanoparticle source. The targets may be arranged concentrically about the axis. At least one of the targets is hollow, and the inlet is arranged to direct a flow of the gas through the hollow target, between at least two of the targets, or both, such that the gas impacts the targets and releases atoms from the targets. The atoms exit the multi-surface nanoparticle source through the second end.
In more detail, inside multi-surface nanoparticle sources, target atoms are ejected from the targets due to the bombardment of argon ions which are generated by the ionization of argon gas (e.g., the supplied sputtering gas). The sputtered atoms form atom gas, and the gas condenses to form nanoparticles. The formed nanoparticles can be carried with a carrier gas and deposited on any suitable substrate of a nanoparticle collection device, including nanoparticle-assembled films.
Sputtering inside the targets and controlling the direction of movement of the nanoparticles can facilitate an automatic nanoparticle collection setup and handling process. Multi-part (e.g., two-part, three-part, or four-part) cooling systems can cool the targets during the sputtering/deposition process.
The systems described in this document can use gas phase condensation techniques based on one or more sputtering sources to fabricate several kinds of nanoparticles, including, but not limited to, heterostructured (e.g., core-shell) nanoparticles such as FeCo—Au, FeCo—SiO2, Fe—Au, Fe—SiO2, Fe5Si3—Au, Fe5Si3—SiO2, and Fe16N2—Fe(N), to name a few examples.
In some cases, the aspect ratio of at least one of the targets is 1:1 or less (e.g., 1:2 or less, 1:4 or less, 1:6 or less, 1:8 or less, 1:10 or less, or 1:16 or less. In certain cases, the aspect ratio is 1:32 or greater. In some examples, the aspect ratio of at least one of the targets is in a range between 1:1 and 1:32 inclusive, in a range between 1:2 and 1:16 inclusive, in a range between 1:4 and 1:10 inclusive, or in a range between 1:6 and 1:8 inclusive.
In certain cases, a multi-surface nanoparticle source includes a magnet proximate the second end of the nanoparticle source. The magnet provides a magnetic field that controls movement of the ionized gas through the nanoparticle source. The magnet may be coupled to an end of one of the targets. In one example, a magnet coupled to an end of a target forms an extension of the target. In some instances, the magnet is a circular or ring magnet having the same inner diameter and outer diameter as the target to which the magnet is coupled. In some instances, the magnet is a circular or ring magnet, and an inner diameter of the ring magnet is greater than the outer diameter of the target to which the circular or ring magnet is coupled. A magnet may include, for example, samarium cobalt, neodymium cobalt, or a combination thereof.
A multi-surface nanoparticle deposition system may include one or more nanoparticle sources (e.g., one or more multi-surface nanoparticle sources) and a nanoparticle collection device housed in a vacuum chamber.
A gas (e.g., argon) can be introduced into a gas inlet 112 at the first end of the nanoparticle source. The gas can be ionized and pass through a plasma region (e.g., nanoparticle-forming region) that is formed by a hollow or open region of the source 104. For example, positively charged ions in the gas can be accelerated by a negative potential at the targets 104A and knock out the atoms of the targets, leading to the formation of atom gas. Then the atom gas can condense to form nanoparticles. In some cases, the nanoparticles crystallize in the thermal environment of the plasma. “Plasma” can refer to the gas that contains formed nanoparticles. The magnetic field 110 can serve to control the movement of the positively charged ions and the formation of the nanoparticles. As a result, erosion of the outside of the source 104 can be minimized, such as at an outlet or second end of the source.
The source 104 includes targets 104A. In some cases, circular magnets 104B are coupled to (e.g., mounted on) the targets 104A or source 104. In some implementations, as shown in
In some implementations, the strength of the magnetic field (or H-field) can be in the range of 970 to 2000 Oe and can depend, for example, on the requirement of nanoparticle growth condition. Magnet selection can also depend on the particle size that is desired for the formed nanoparticles. Longer targets can increase the crystallization time and produce larger nanoparticles. Thicker magnets can increase the growth time and produce larger nanoparticles. In this example, the multi-tube target source 104A and the circular magnets 104B are made from tubes, which may be advantageous in terms of manufacturing the components, but in some implementations other shapes can be used.
The targets 104A have the same potential on all tubes in this example. For example, having one anode and one cathode may not be suitable.
Generally, the properties and applications of fabricated nanoparticles will typically be determined by particle size and its crystal structure. For example, the field strength affects the intensity of the plasma, and the magnet length affects the length (L in the figure) of the plasma. The plasma's intensity and length, moreover, can determine the nanoparticles' size and phase. This indicates the plasma heating effect supplied by the magnet assembly.
Based on this calculation result, a P·D0.1 of 290 Pa-mm is obtained. In terms of distance, half of the gap between tube targets in the nanoparticle source was here used. In this example, D0.1=2.5 mm, and P·D0.1=290 Pa-mm, which gives P≧780 mTorr as the pressure required for formation of nanoparticles via sputtering.
Assuming that the sputtering current density is constant, the nanoparticle yield rate will be proportional to the area of the target's sputtered surface, for example according to the following equation:
R=(0.0557mg/hr/cm2)·S,
where R is the nanoparticle yield rate and S is the area of the target's sputtered surface.
Table 1 lists estimated nanoparticle yield rates using a multi-tube source having a target length of 4 cm, and four concentric tube targets. ID and OD stand for inner and outer diameters, respectively, of the tubes that define the gap. For example, the first gap is defined by the outer diameter of the smallest tube target, and by the inner diameter of the next smallest tube target. Because the ID−OD difference of adjacent targets is 1 cm, the gap distance used in this example is 5 mm.
The numbers above can be contrasted with, for example, a single-tube source. Table 2 provides an estimated nanoparticle yield rate for a single-tube source with a target length of 4 cm.
The multi-tube source 104 can be manufactured with different dimensions. For example, a 5 mm gap is used in the above estimations. In some implementations, 2 mm may be a lower limit for the gap size, because with too small a gap it will be difficult for the material to exit the target. On the other hand, if too large a gap is used, its dimension begins to compete with the overall length of the target. For example, this can occur with 10-15 mm gaps, or larger. The target can have a ratio of gap distance, or ½|OD−ID| for adjacent targets to the target length of (i.e., an aspect ratio) of 1:1 or less (e.g., 1:2 or less, 1:4 or less, 1:8 or less, or 1:16 or less). In one example, with a 4 cm tube length and a 5 mm gap, the aspect ratio is 1:8.
The multi-tube target source 104A can be segmented.
The width of the segments 402 and/or 404 can be determined by the composition that is desired. For example, less Au as the shell and more FeCo as the core, can be obtained. The proportions of the segments 402 and 404 do not necessarily determine the ratio of materials in the nanoparticles. For example, the materials can have different deposition rates.
In another implementation, the second material can include SiO2. For example, this can be used to generate FeCo—SiO2 core-shell structure nanoparticles.
In another implementation, the second material can include SiO2. For example, this can be used to generate FeCo—SiO2 core-shell structure nanoparticles.
The system 800 includes one or more nanoparticle sources 804. In some implementations, the nanoparticle source 804 can include one or more segments, such as 804A and B. For example, the segment 804A can be formed of one material (e.g., FeCo) and the segment 804B can be formed of a second material (e.g., Au or SiO2.)
The nanoparticle source 804 has one or more openings 806.
The opening(s) 806 can have any suitable shape. In some implementations, the opening has a linear configuration. This can be useful for coating a continuous tape substrate that is used for collecting the deposited nanoparticles. For example, and without limitation, the opening can have a 5 mm opening width (e.g., “x-axis”) and an opening height of one or more centimeters (e.g., “y-axis.”) In some implementations, an opening width of several centimeters can provide good conditions for maintaining the plasma for sputtering. For example, the deposition rate proportional to the surface area of the deposition system can be increased. Using two or more openings 806 can further increase the deposition rate. For example, a source array of multiple nanoparticle sources 804 can be used.
The multi-surface nanoparticle deposition system 900 includes an insulator 1000. For example, a 4.5″ insulator can be used.
The system 900 includes at least one tube 1002. For example, three telescoping tubes can be used.
The system 900 includes a vacuum tube brace assembly 1004. For example, any of the target and/or magnet configurations described herein can be used.
The system 900 includes a tube 1006. For example, a vacuum gauge tube can be used.
The system 900 includes a gas supply 1008. For example, a gas supply tube weldment can be used.
The system 900 includes a nanoparticle source 1010. The nanoparticle source may be any nanoparticle source described herein.
The system 900 includes a base plate weldment 1012. For example, any suitable shape and/or material can be used for the base plate weldment.
The system 900 includes at least one tubing support spacer 1014. For example, two tubing support spacers of any suitable shape and/or material can be used.
The system 900 includes at least one tube 1016. For example, two water extension tubes can be used.
The system 900 includes a power supply 1018. For example, any suitable power wire can be used for the power supply.
The system 900 includes at least one gas tube 1020. For example, two gas tubes of any suitable shape and/or material can be used.
The system 900 includes at least one gas tube support 1022. For example, any suitable shape and/or material can be used for the gas tube support.
The system 900 includes a movement weldment 1024. For example, any suitable shape and/or material can be used for the movement weldment.
The system 900 includes a nut 1026. For example, a 2″-12 nut can be used.
The system 900 includes a disconnect 1028. For example, a quick disconnect can be used.
The cooling block 1402 and multiple tube targets 1404 form a multi-tube source 1406. The targets 1404, one of which is shown individually for clarity, are tube sputtering targets made from a suitable material, including, but not limited to, FeCo and Au. That is, the cooling block has multiple openings, and a tube sputtering target can be inserted in each opening. In some implementations, each tube sputtering target behaves in the same or a similar way as a single-tube nanoparticle deposition source. For example, the total deposition rate of the multi-tube source may be equal to the deposition rate of a single source multiplied by the number of openings.
The targets 1404 can be arranged on the cooling block 1402 in any suitable orientation or location. In some implementations, the targets are placed in a regular pattern. For example, the targets 1404 here form a first ring 1408A and a second ring 1408B positioned concentrically about an axis that extends from a first end of source 1406 (e.g., the inlet) to a second end of the source (e.g., the outlet). The system 1400 can include one or more circular magnets (not shown) coupled to or positioned proximate the tube targets. For example, a multi-tube magnet can be used with the multi-tube source 1406.
The multi-surface nanoparticle deposition system 1400 can be cooled in one or more ways. In some implementations, at least one fluid can be brought in thermal contact with some or all of the targets 1404. Here, for example, the cooling block 1402 includes one fluid inlet 1410A and at least one fluid outlet 1410B, with a cooling chamber therebetween in the cooling block. Any suitable fluid can be used, including, but not limited to, water.
As with other nanoparticle sources described herein, an aspect ratio of at least one of the targets is 1.1 or less. For tube targets such as tube target 1404, the aspect ratio is calculated as the ratio of the diameter of the opening to the length of the target.
Table 3 lists estimated nanoparticle deposition rates for a system in which each tube target has diameter 0.5 cm and length 4 cm. For example, such estimation can be relevant to the targets 1404, such as in an integrated multi-surface nanoparticle deposition system using cylindrical configuration (e.g., system 1400).
One or more spaces 1708 can be formed between adjacent cooling blocks. For example, the space 1708 can facilitate energy dissipation from the cooling block(s) to the environment, and/or facilitate thermal isolation between two or more cooling blocks. In some implementations, the space(s) 1708 can be partially or completely filled with a thermally insulating material. In this example, the space 1708 is essentially cylindrical.
The multi-tube target 2004 can include multiple targets, such as the targets 1404. The targets 1404 can be arranged on the multi-tube target 2004 in any suitable orientation or location. The targets can be placed in a regular pattern, for example in essentially circular arrangement about axis c. In some implementations, the multi-surface target 2002 is considered a large tube sputtering target and the targets 1404 are considered a small tube sputtering target.
The multi-surface target 2002 and/or the multi-tube target 2004 can be provided with cooling. In some implementations, the tube 2006A has fluid inlet 2010A and fluid outlet 2010B, and the tube 2006B has fluid inlet 2012A and fluid outlet 2012B. In some implementations, one or more targets 1404 can be placed in the space 2008.
Table 4 lists estimated nanoparticle deposition rates for a system in which each tube target has diameter 0.5 cm and length 4 cm. For example, such estimation can be relevant to the targets 1404, such as in an integrated multi-surface nanoparticle deposition system using cylindrical configuration (e.g., system 2000).
The multi-surface nanoparticle deposition system 2300 can be cooled in one or more ways. In some implementations, at least one fluid can be brought in thermal contact with some or all of the targets 1404. Here, for example, the cooling block 2302 includes one fluid inlet 2304A and at least one fluid outlet 2304B. Any suitable fluid can be used, including, but not limited to, water.
Table 5 lists estimated nanoparticle deposition rates for a system in which each tube target has diameter 0.5 cm and length 4 cm. For example, such estimation can be relevant to the targets 1404, such as in an integrated multi-tube nanoparticle deposition system using a cube configuration (e.g., having a square shape in the front, such as system 2300).
The magnetic field supply can form one or more coils 2906 around the source 2904. For example, the coil can have at least one current inlet 2908A and at least one current outlet 2908B. In some implementations, a combination of a cooling block and coil(s) can behave as an electromagnet which can generate a large magnetic field inside each tube target. The arrangement using a coil (e.g., the magnetic field supply 2902) can be used with some or all systems described herein.
In some implementations, one or more rotating magnetron sources can be used for nanoparticle deposition. For example, rotating magnets or rotating electromagnets can provide a magnetic field to different areas of a single target or to multiple targets such as targets arranged in a circle.
In some implementations, multi-source integrated nanoparticle deposition system can funnel particles of different types through a magnetic field to a substrate or compression die. As a result, particles having different characteristics can be manufactured and collected simultaneously.
A number of implementations have been described. Nevertheless, it will be understood that various modifications may be made without departing from the spirit and scope of this disclosure.
This application claims priority to U.S. Appl. Ser. No. 61/759,678 entitled “MULTI-SURFACE NANOPARTICLE DEPOSITION SYSTEMS,” filed on Feb. 1, 2013, which is incorporated herein by reference in its entirety.
Filing Document | Filing Date | Country | Kind |
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PCT/US2014/014264 | 1/31/2014 | WO | 00 |
Number | Date | Country | |
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61759678 | Feb 2013 | US |