Ultrahigh vacuum instrument for molecular beam epitaxy
A portable, compact UHV instrument with passive pumping and advanced synthesis capabilities addresses the limitations of existing UHV transport solutions, enabling efficient, low-cost, and reliable UHV conditions for materials research and synthesis.
Patent Information
- Application Number
- PCT/US2024/041463
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2023-08-08
- Filing Date
- 2024-08-08
- Publication Date
- 2025-02-13
AI Technical Summary
Existing ultrahigh vacuum (UHV) transport solutions are heavy, complex, and limited in capacity, leading to high costs and failure rates due to contamination and degradation during transportation, and require extensive recipe iteration across different UHV systems.
A portable, compact UHV instrument with passive pumping capabilities, capable of maintaining UHV conditions for extended periods without electrical power, and equipped with features such as non-evaporable getter pumps, ion pumps, sputtering guns, and gas-dosing capabilities for on-the-go sample synthesis and reinvigoration.
The solution enables practical, low-cost portability of UHV equipment, allowing for extended UHV conditions and efficient sample synthesis and characterization across different systems, significantly reducing costs and improving the reliability of materials research and synthesis.
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Figure US2024041463_13022025_PF_FP_ABST
Abstract
Description
ULTRAHIGH VACUUM INSTRUMENT FOR MOLECULAR BEAM EPITAXYCROSS-REFERENCE TO RELATED APPLICATIONS
[0001] This application claims the benefit of U.S. Provisional Application No. 63 / 531,338, filed August 8, 2023, which is incorporated by reference as if disclosed herein in its entirety.FIELD
[0002] The present technology relates to ultrahigh vacuum instruments (UHV) and, in particular, to UHV systems with improved portability and functionality for material engineering and synthesis.BACKGROUND
[0003] Modem layer-by-layer materials engineering almost always requires an UHV synthesis environment. Materials synthesized in a UHV chamber can be easily contaminated if exposed to regular high or rough vacuum or atmospheric pressure during the process of transportation to different equipment for characterization and processing.
[0004] In addition, UHV synthesis recipes for the same material are known to vary from one UHV chamber to another due to differences in the characteristics of the chambers.Refinement of the synthesis condition from chamber to chamber is usually time-consuming and / or very costly.
[0005] Existing in-situ UHV suitcases, which are often used to transport layer-by-layer materials, 1) are extremely heavy and complex to operate, and 2) offer limited capacity for transferring samples under vacuum conditions between different UHV systems. Further, if the transportation time is beyond one or two days, or these samples fail via degradation or contamination, existing UHV suitcases have no capacity to “reinvigorate” these samples. Therefore, existing UHV transport solutions offer a one-shot opportunity for those often high- cost, high stakes operations coordinated across multiple industry / research sites. Given the high failure rate and the inherent requirement of recipe iteration, the cost associated with each successful experiment is very high for the materials and travel alone.
[0006] Standard materials syntheses systems such as molecular beam epitaxy (MBE), physical vapor deposition (PVD), and chemical vapor deposition (CVD) can synthesize samples with high quality, but the physical equipment often weighs tons, and are therefore impractical to move around to accommodate additional processing or characterization in another disconnected system. Moreover, the growth receipt for the same materials varies from system to system, which makes the synthesis of the same materials in different systems time-consuming.
[0007] What is needed, therefore, is UHV equipment that enables practical, low-cost portability. What is also needed is UHV equipment that provides a UHV synthesis environment. What is further needed is UHV equipment that provides extended UHV conditions even in the absence of electrical power.SUMMARY
[0008] Embodiments of the present technology seek to address one or more of the foregoing needs. Some embodiments provide a portable, compact UHV environment to store, transport, and manipulate thin film samples with passive pumping (i.e., no power is needed to maintain UHV). Some embodiments provide a portable UHV synthesis setup by shrinking the footprint of a typical molecular beam epitaxy (MBE) setup by more than 20x.
[0009] Some embodiments provide a portable UHV-compatible material synthesis instrument with UHV holding capability for long periods of time without needing any active power input using one or both of a non-evaporable getter pump and an ion pump. Some embodiments provide the ability to perform UHV layer-by-layer sample synthesis on-the-go, and to reinvigorate the material if degradation occurs. Some embodiments include a heater that can anneal the sample to remove surface adsorptions. Some embodiments include at least one sputtering gun that can sputter the sample surface to get a clean and atomically flat surface.Some embodiments have one or more ports to integrate at least one evaporating source to grow materials in situ. Some embodiments include gas-dosing capabilities to carry out chemical vapor deposition for materials synthesis or chemical reactions. In some embodiments, gas-dosing capabilities include enabling chemical reactions to decorate, clean, or change target samples.
[0010] According to one embodiment of the present technology, a UHV instrument is provided that comprises a vacuum chamber; a first valve for opening and closing the vacuum chamber, and adapted to connect to at least one other vacuum instrument; a sample storage stage insertable into the vacuum chamber to position a sample in the vacuum chamber; at least one of a non-evaporable getter and ion pump connected to the vacuum chamber to reduce the ambient pressure in the vacuum chamber; a motion stage coupled to the sample storage stage for changing the position of the sample storage stage; and a first vacuum port adapted to connect to at least one of a sputtering gun for cleaning a sample surface or an evaporator for supplying material to grow a film on a sample
[0011] According to a second embodiment of the present technology, a sample storage stage for a UHV instrument is provided, comprising: a first sample parking position; a heating element adapted to apply heat to a sample loaded in the first sample parking position; one or more second sample parking positions; and a thermal insulating plate positioned to insulate the second sample parking positions from heat generated by the heating element.
[0012] Further objects, aspects, features, and embodiments of the present technology will be apparent from the drawing Figures and below description.BRIEF DESCRIPTION OF THE DRAWINGS
[0013] Some embodiments of the present technology are illustrated as an example and are not limited by the figures of the accompanying drawings, in which like references may indicate similar elements.
[0014] FIGs. 1 A and IB each show a perspective view of an UHV instrument according to a first embodiment of the present technology.
[0015] FIG. 1C shows a cross-section side view of the UHV instrument according to FIGs. lA and IB.
[0016] FIG. 2A shows a perspective view of a sample store stage according to an embodiment of the present technology.
[0017] FIG. 2B shows a perspective view of a portion of the sample storage stage of FIG.2A.
[0018] FIG. 2C shows an exploded view of a sample parking position, heating element, and thermal insulating plate of the sample storage stage of FIG. 2B.
[0019] FIG. 3 shows a perspective view of a UHV instrument according to a second embodiment of the present technology
[0020] FIG. 4 shows a perspective view of a UHV instrument according to a third embodiment of the present technology.
[0021] FIG. 5 shows a flowchart of a method of using a UHV instrument according to an embodiment of the present technology.
[0022] FIGs. 6A and 6B show flowcharts of methods of using a sample storage stage according to embodiments of the present technology.DETAILED DESCRIPTION
[0023] In the modern semiconductor industry and solid-state materials research sectors, the synthesis of high-quality, scalable thin film materials often relies on sophisticated scientific instruments. The associated capital instrument cost (not including maintenance) for molecular beam epitaxy (MBE), physical vapor deposition (PVD), and chemical vapor deposition (CVD) instruments can be millions of dollars. Further, the typical weight of such instruments is often a half-ton or more such that they must be confined to one laboratory. In general, instrument versatility (i .e., the variety of materials that can be grown) requires an expensive and heavy machine. Further, the typical procedures to optimize the best recipes for high-quality materials synthesis in such sophisticated systems can take several months if not years. In most cases, the best recipes for high-quality materials synthesis also vary from system to system, which makes the replication of the same materials in a different system a daunting, if not impossible, task. Some embodiments of the present technology relate to instruments that are both highly portable and highly versatile.
[0024] Figures 1 A, IB, and 1C show a first embodiment of an UHV instrument 100 according to the present technology. The instrument 100 comprises a vacuum chamber 101 and a first valve 102 for opening and closing the vacuum chamber and adapted to connect to at least one other vacuum instrument. In some embodiments, the first valve 102 comprises connection hardware to enable connection to another instrument, including another UHV instrument. In some embodiments, the connection hardware comprises a flange 103 with bolt holes 104. The other UHV instrument is connected via a corresponding flange with a gasket (such as a copper gasket) compressed between the flanges. In some embodiments, the first valve 102 comprises a gate valve that is manually operated in some embodiments and pneumatically operated in other embodiments.
[0025] The instrument 100 also includes a sample storage stage 105, which is shown in the cutaway view in FIG. 1C and in detail in FIGs. 2A and 2B. The sample storage stage is insertable into the vacuum chamber to position a sample in the vacuum chamber. As described in further detail below, some embodiments include hardware 108 for heating a sample held in the sample storage stage 105.
[0026] The instrument 100 further includes at least one of a non-evaporable getter (NEG) and ion pump 106 connected to the vacuum chamber 101 to reduce the ambient pressure in the vacuum chamber 101 . In some embodiments, only a non-evaporable getter is included in the instrument for reducing the ambient pressure in the vacuum chamber. In still other embodiments, only an ion pump is included. In some embodiments, the NEG / pump 106 comprises an integrated non-evaporable getter and ion pump. In some embodiments, the integrated non-evaporable getter and ion pump 106 can maintain the chamber pressure below 10"9mbar. In some embodiments, the NEG and ion pump 106 will maintain this pressure for more than 7 days. FIG. 1 A also shows a pump valve 107 by means of which the non-evaporable getter and / or ion pump can be sealed. Pump valve 107 comprises a pneumatic or manual gate valve in some embodiments.
[0027] The instrument shown in FIGs. 1A-1C further comprises a motion stage 109 that is coupled to the sample storage stage 105 for changing the position of the sample storage stage. In some embodiments, the motion stage 109 is a linear motion stage that is coupled to the samplestorage stage via a magnetic coupling. Tn some embodiments, the linear motion stage 109 enables movement of the sample storage stage along a longitudinal axis 206 (as shown in FIG. 2A) of the sample storage stage. This enables the sample(s) in the sample storage stage 105 to be moved to different positions along a linear axis in the vacuum chamber 101. In some embodiments, the motion stage 109 also includes rotary motion capability to enable rotation of the sample stage within the vacuum chamber.
[0028] The instrument 100 further comprises a first vacuum port 110 adapted to connect to a sputtering gun for cleaning a sample surface or an evaporator for supplying material to grow a film on a sample. In some embodiments, the port 110 includes connection hardware for connecting to a sputtering gun or evaporator that comprises a flange and a plurality of bolt holes. The flange and bolt holes correspond to a flange on the sputtering gun or evaporator that is bolted to the port using a gasket, such as a copper gasket. A sputtering gun enables cleaning of the sample by ions.
[0029] In some embodiments, the instrument 100 further comprises a transfer rod 111, by means of which the sample position can be changed along an axis that is different than the axis along which the linear motion stage moves. In some embodiments, the transfer rod 111 enables movement of samples along an axis that is perpendicular to the axis along which they are moved via the motion stage 109. In some embodiments, the transfer rod 111 also enables a sample to be moved from the vacuum chamber 101 to a separate instrument, such as a second UHV instrument. In such a situation, the sample would be secured by a coupling device, removed from the sample storage stage 105, and moved out of the chamber 101 via the valve 102. In some embodiments, the coupling device on the transfer arm utilizes magnetic force to couple to and move the sample. In some embodiments, the transfer arm is foldable to reduce the overall dimension of the instrument 100, including by hinges. In some embodiments, the transfer arm includes telescoping components to reduce the overall dimension of the instrument 100.
[0030] In the embodiment shown in FIGs. 1A-1C and in some other embodiments, the instrument includes a second and third vacuum ports 112, 113 each adapted to connect to a sputtering gun or an evaporator for materials deposition. In some embodiments, the evaporator comprises a resistance-heating evaporator or an electron beam heating evaporator. In someembodiments, the instrument includes a fourth vacuum port, and each of the first, second, third, and fourth vacuum ports are adapted to connect to a sputtering gun or to a four-source evaporator for supplying material to grow a film on a sample simultaneously.
[0031] In some embodiments, as shown in FIGs. 1 A-1C, the instrument 100 also includes one or more valve ports, each connected to a leak valve and a gas cylinder for supplying one or more gases to the vacuum chamber 101. For example, a first valve port 118 is connected to a first leak valve 114 and a first gas cylinder 115 for supplying a first gas to the vacuum chamber 101. In some embodiments, the first gas is argon for the sputtering gun. In some embodiments, the first gas is neon for the sputtering gun. In some embodiments, the first gas is krypton for the sputtering gun.
[0032] In some embodiments, the vacuum chamber 111 of the instrument includes a second valve port 119 connected to a second leak valve 116 and a second gas cylinder 117 for supplying a second gas to the vacuum chamber 101. In some embodiments, the second gas cylinder supplies gas for chemical vapor deposition synthesis of samples or other chemical reactions on a sample in the vacuum chamber 101. In some embodiments, the gases in the first and second gas cylinders are exchangeable for different species of gas. In some embodiments, the first and second leak valves regulate gas dosing pressure from between approximately 10’10Torr to approximately 1 O'4Torr.
[0033] FIGs. 2A and B, show an embodiment of a sample storage stage 105, with FIG. 2B showing a close-up view of a bottom portion of the stage 105. The sample storage stage 105 comprises a first sample parking position 201, in which a sample 202 (such as a flag-type sample plate) can be held for material deposition or other processes within the vacuum chamber 101. The sample storage stage 105 also includes, in some embodiments, a heating element 203 adapted to apply heat to a sample loaded in the first sample parking position 201. In some embodiments, the sample storage stage 105 includes one or more second sample parking positions 204. In some embodiments, the components that make up the sample parking positions are formed of aluminum alloys, stainless steel, titanium, bronze, or other materials suitable for UHV process conditions. In this embodiment, a sample storage stage 105 consists of multiple second sample parking positions 204. In this embodiment, there are a total of four secondsample parking positions 204, and they are arranged in a stacked relationship to each other. In other embodiments, more or fewer parking positions are included. FIG. 2A shows flag-type sample plates 211 parked in the second sample parking positions 204, while FIG. 2B shows these parking positions vacant.
[0034] In some embodiments, the sample storage stage 105 includes a thermal insulating plate 205 positioned to insulate the second flag-type sample parking positions 204 from heat generated by the heating element 203. In this and some other embodiments, the thermal insulating plate is disposed between the heating element 203 and the second sample parking positions 204. In some embodiments, multiple samples can thus be stored at room temperature on the second flag-type sample holders while the front end performs high temperature sample annealing and surface regeneration to a sample in the first sample holder 201. In some embodiments, the heating element 203 comprises a filament through which electrical current flows to heat a sample. In some embodiments, the heating element 203 enables the sample in the chamber to be annealed up to about 1000°C, in some embodiments. In other embodiments, the heating stage enables the sample to be annealed up to about 850°C. In still other embodiments, the filament can heat a sample up to about 900°C.
[0035] In some embodiments, the first and second sample parking positions 201, 204 are adapted to hold flag-type sample plates. In other embodiments, other types of sample plates and sample holders are used. In some embodiments, the first sample parking position 201, heating element 203, thermal insulating plate 205, and second sample parking positions 204 are arranged in a stacked relationship, as shown in FIGs. 2A and 2B. In the embodiment shown and some other embodiments, the first sample parking position 201 are positioned on a bottom end of the sample storage stage, meaning that the first sample parking position 201 is lowered along axis 206 into the vacuum chamber 101.
[0036] In some embodiments, the second sample parking positions 204 are secured to a vacuum feedthrough flange 207 by one or more first frames 208. In some embodiments, the first frames 208 are rods, such as cylindrical rods. In some embodiments, the first sample parking position 201, heating element 203, and thermal insulating plate 205 are secured to the second sample parking positions 204 by one or more second frames 209. In the embodiment shown andin some other embodiments, the second frames 209 are rods, such as cylindrical rods. Tn some embodiments, such as the embodiments shown, first and second rods are separate components to limit heat transmission from the first sample parking position 201, the heating element 203, and insulating plate 205 to the second parking positions 204. In some embodiments, the second sample parking positions 204 are secured to a vacuum feedthrough flange 207 by three first frames 208, and wherein the first sample parking position 201, heating element 203, and thermal insulating plate 205 are secured to the second sample parking positions 204 by three second frames 209.
[0037] In some embodiments, the sample storage stage 105 further comprises an electrical feedthrough 210 (i.e., a vacuum-air electrical feedthrough) for providing electrical current through the vacuum feedthrough flange 207 to the heating element 203 and for receiving a thermocouple temperature measurement signal from the heater.
[0038] FIG. 2C shows an exploded view of the sample stage 105, including the first sample parking position 201, the heating element 203, the thermal insulating plate 205, and the thermocouple leads 212.
[0039] Various embodiments of UHV instruments according to the present technology have different groups of features to provide varying levels of functionality and instrument cost. For example, base or lower-cost model instruments can have a small form factor and high portability relative to the other UHV instrument embodiments that have additional features. Instrument 100 as shown in FIGs. 1 and 2 is a mid-level, standard model with 3-4 element synthesis capabilities, cross-platform sample transfer compatibility, and sputter-anneal substrate treatment capability.
[0040] By contrast, FIG. 3 shows instrument 300, which has the core functionality of single-element thin-film synthesis and substrate thermal treatment, and provides a base or lower- cost model. Instrument 300 includes a vacuum chamber 301; a valve 302 by means of which the chamber can be opened or closed and attached to different vacuum instruments. The instrument 300 also includes an integrated heater and sample store stage 305 / 308, (such as the stage shown in FIGS. 2A-2C) by means of which a sample in the chamber can be annealed up to about 1000°C and multiple samples can be stored in the chamber.
[0041] A motion stage 309 enables the position of the integrated heater and sample store stage to be changed, and a transfer rod 311 for changing the sample position and / or moving a sample out of the chamber 301 and into a second instrument. This embodiment also includes a non-evaporable getter and ion pump 306 to maintain the chamber pressure below about 10'9mbar. This embodiment includes a second valve 307 for sealing the non-evaporable getter and ion pump and an additional vacuum port 310 to accommodate a sputtering gun to clean sample surface and / or an evaporator to grow fdms.
[0042] FIG. 4 shows an embodiment an upper-level instrument 400, with additional features beyond those included in instrument 100. Instrument 400 is an upper-level model featuring up to 12 element synthesis, a foldable transfer arm, chemical vapor deposition compatibility, and a larger passive pump to maintain better vacuum for longer time (for example, about 4-6 days without power, in some embodiments). The instrument 400 includes a vacuum chamber 401 and a valve 402 for opening and closing the chamber and attaching to different vacuum instruments. This embodiment also includes an integrated heater and sample store stage 405 / 408, by means of which a sample in the chamber can be annealed up to about 1000°C and multiple samples can be stored in the chamber. A motion stage 409 is provided for changing the position of the integrated heater and sample store stage. A transfer rod 411 is also included for changing the sample position and moving a sample to a second instrument attached at valve 402. The instrument 400 also includes a non-evaporable getter and ion pump 406 to maintain the chamber pressure below about 10'9mbar and a second valve 407 by means of which the non- evaporable getter and ion pump can be sealed.
[0043] This embodiment includes four additional vacuum ports 410 to accommodate, for example, one sputtering gun to clean sample surface and three four-source evaporators to grow up to 12 kinds of films. In this embodiment, two gas bottles 415 are coupled to the UHV chamber 401 : one gas cylinder can be used to supply argon for the sputtering gun, for example, and a second gas cylinder to supply gas for chemical vapor deposition synthesis of samples or other chemical reactions on the sample. The gas is regulated in this embodiment by two leak valves 414, which regulate the gas dosing pressure from about 10’10Torr to about 10'4Torr range.
[0044] Accordingly, some embodiments of the present technology include UHV instruments that weigh less than 15 kg and that can store and transfer samples under UHV conditions between different UHV instruments at vastly different geolocations. Some embodiments include a sample storage stage that can accommodate up to 5 different thin film samples. In some embodiments, the sample storage stage includes a compact heater to degas samples at up to about 800° Celsius, about 900° Celsius, or, in some embodiments about 1000° Celsius. Some embodiments include a non-evaporable getter pump (passive, no need to be powered) and / or an ion pump (active, needs to be powered) to maintain the UHV condition down to 10'10mbar for more than 100 hours in some embodiments. In some embodiments, an ion source is included to sputter samples so that an atomically flat sample surface over a mm-scale lateral dimension can be achieved.
[0045] The present technology also includes methods of using some embodiments of a UHV instrument described herein to grow a film on a target sample. As shown in FIG. 5, one embodiment of such a method 500 includes the steps of: cleaning the target sample surface with a sputtering gun at 501; heating the target sample to flatten the surface at 502; evaporating a target film material to enable growth of a target film on the target sample surface at 503; and connecting at least one external vacuum system for additional sample processing at 504. In some embodiments, additional sample processing includes taking measurements of one or more sample characteristics. In some embodiments, the steps of cleaning and heating the target sample are repeated until an atomically flat sample surface is achieved.
[0046] The present technology also includes methods of using embodiments of a sample storage stage for an ultra-high vacuum instrument described herein. As shown in FIG. 6A and 6B, one embodiment of such a method 600 includes the steps of: loading a target sample in the first sample parking position at 601; growing at least one target film on the target sample at 602; and transferring the target sample to one of the second sample parking positions at 603. In some embodiments, the step of growing at least one target film comprises the steps of: cleaning the target sample surface with a sputtering gun at 604; heating the target sample to flatten the surface at 605; and evaporating a target film material to enable growth of a target film on the target sample surface 606. In some embodiments, the target sample is disposed on a flag-type sample plate. In some embodiments, the method further comprises repeating the steps of loading,growing, and transferring for a plurality of target samples until each of the one or more second sample parking positions contains a target sample.
[0047] In addition to the function of transferring multiple samples under UHV conditions, some embodiments of the current technology can revive the transferred samples via a full suite of on-site and in-situ operations such as annealing, sputtering, gas dosing, and deposition. Thus, some embodiments provide “infinite” sample tunability between different systems. Because all the samples are treated and synthesized in the same portable UHV chamber, all related best recipes stay the same and make the revival / regrow process highly repeatable and more efficient. Portable materials synthesis instruments according to some embodiments of the present technology include modern materials synthesis technologies, but a reduced size, weight, and cost by more than 20 times in some cases. Therefore, once the best materials synthesis recipe is optimized in some embodiments according to this technology, it can be connected with different characterization systems and continuously grow the same materials, and study different properties. Together with its ability to transfer multiple samples, some embodiments of the present technology can greatly speed up the materials research frontier by bridging differently advanced UHV characterization systems and continuously supplying target materials.
[0048] As will be apparent to those skilled in the art, various modifications, adaptations, and variations of the foregoing specific disclosure can be made without departing from the scope of the technology claimed herein. The various features and elements of the technology described herein may be combined in a manner different than the specific examples described or claimed herein without departing from the scope of the technology. In other words, any element or feature may be combined with any other element or feature in different embodiments, unless there is an obvious or inherent incompatibility between the two, or it is specifically excluded.
[0049] References in the specification to “one embodiment,” “an embodiment,” etc., indicate that the embodiment described may include a particular aspect, feature, structure, or characteristic, but not every embodiment necessarily includes that aspect, feature, structure, or characteristic. Moreover, such phrases may, but do not necessarily, refer to the same embodiment referred to in other portions of the specification. Further, when a particular aspect, feature, structure, or characteristic is described in connection with an embodiment, it is withinthe knowledge of one skilled in the art to affect or connect such aspect, feature, structure, or characteristic with other embodiments, whether or not explicitly described.
[0050] The singular forms "a," "an," and "the" include plural reference unless the context clearly dictates otherwise. Thus, for example, a reference to "a plant" includes a plurality of such plants. It is further noted that the claims may be drafted to exclude any optional element. As such, this statement is intended to serve as antecedent basis for the use of exclusive terminology, such as "solely," "only," and the like, in connection with the recitation of claim elements or use of a "negative" limitation. The terms “preferably,” “preferred,” “prefer,” “optionally,” “may,” and similar terms are used to indicate that an item, condition, or step being referred to is an optional (not required) feature of the technology.
[0051] The term "and / or" means any one of the items, any combination of the items, or all of the items with which this term is associated. The phrase "one or more" is readily understood by one of skill in the art, particularly when read in context of its usage.
[0052] Each numerical or measured value in this specification is modified by the term “about.” The term "about" refer to a variation of ± 10%, of the value specified unless stated otherwise. Unless indicated otherwise herein, the term "about" is intended to include values and ranges proximate to the recited range that are equivalent in terms of the functionality of the composition, or the embodiment.
[0053] As will be understood by one skilled in the art, for any and all purposes, particularly in terms of providing a written description, all ranges recited herein also encompass any and all possible sub-ranges and combinations of sub-ranges thereof, as well as the individual values making up the range, particularly integer values. A recited range (e.g., weight percents of carbon groups) includes each specific value, integer, decimal, or identity within the range. Any listed range can be easily recognized as sufficiently describing and enabling the same range being broken down into at least equal halves, thirds, quarters, fifths, or tenths. As a non-limiting example, each range discussed herein can be readily broken down into a lower third, middle third, and upper third, etc.
[0054] As will also be understood by one skilled in the art, all language such as "up to," "at least," "greater than," "less than," "more than," "or more," and the like, include the number recited and such terms refer to ranges that can be subsequently broken down into sub-ranges asdiscussed above. In the same manner, all ratios recited herein also include all sub-ratios falling within the broader ratio. Accordingly, specific values recited for radicals, substituents, and ranges, are for illustration only; they do not exclude other defined values or other values within defined ranges for radicals and substituents.
[0055] One skilled in the art will also readily recognize that where members are grouped together in a common manner, such as in a Markush group, the technology encompasses not only the entire group listed as a whole, but each member of the group individually and all possible subgroups of the main group. Additionally, for all purposes, the technology encompasses not only the main group, but also the main group absent one or more of the group members. The technology therefore envisages the explicit exclusion of any one or more of members of a recited group. Accordingly, provisos may apply to any of the disclosed categories or embodiments whereby any one or more of the recited elements, species, or embodiments, may be excluded from such categories or embodiments, for example, as used in an explicit negative limitation..
Claims
CLAIMSWe claim:
1. An ultra-high vacuum instrument, comprising: a vacuum chamber; a first valve for opening and closing the vacuum chamber, and adapted to connect to at least one other vacuum instrument; a sample storage stage insertable into the vacuum chamber to position a sample in the vacuum chamber; at least one of a non-evaporable getter and ion pump connected to the vacuum chamber to reduce the ambient pressure in the vacuum chamber; a motion stage coupled to the sample storage stage for changing the position of the sample storage stage; and a first vacuum port adapted to connect to at least one of a sputtering gun for cleaning a sample surface or an evaporator for supplying material to grow a film on a sample.
2. The instrument of claim 1, further comprising that the at least one of the non-evaporable getter and ion pump comprises an integrated non-evaporable getter and ion pump.
3. The instrument of any of claims 1-2, wherein the sample storage stage comprises: a first sample parking position; a heating element adapted to apply heat to a sample loaded in the first sample parking position; one or more second sample parking positions; and a thermal insulating plate positioned to insulate the second flag-type sample parking positions from heat generated by the heating element.
4. The instrument of claim 3, wherein the heating element comprises a filament through which electrical current flows to heat a sample.
5. The instrument of any of claims 3-4, wherein the first and second sample parking positions are adapted to hold flag-type sample plates, and the first sample parking position,heating element, thermal insulating plate, and second sample parking positions are arranged in a stacked relationship.
6. The instrument of any of claims 3-5, wherein the second sample parking positions are secured to a vacuum feedthrough flange by one or more first frames, and wherein the first sample parking position, heating element, and thermal insulating plate are secured to the second sample parking positions by one or more second frames.
7. The instrument of any of claims 3-6, further comprising an electrical feedthrough for providing electrical current through the vacuum feedthrough flange to the heating element and for receiving a thermocouple temperature measurement signal from the heater.
8. The instrument of any of claims 1-7, further comprising a second vacuum port and a third vacuum port each adapted to connect to a sputtering gun for cleaning a sample surface or an evaporator for supplying material to grow a film on a sample.
9. The instrument of claim 2, further comprising a fourth vacuum port, and wherein each of the first, second, third, and fourth vacuum ports are adapted to connect to a sputtering gun or to a four-source evaporator for supplying material to grow a film on a sample simultaneously.
10. The instrument of any of claims 1-9, wherein the vacuum chamber further comprises one or more valve ports, each connected to a leak valve and a gas cylinder for supplying one or more gases to the vacuum chamber.
11. The instrument of claim 10, wherein each gas cylinder is exchangeable for an alternative gas cylinder containing a different species of gas.
12. The instrument of any of claims 10-11, wherein at least one of the leak valves regulates gas dosing pressure from between approximately I O'10Torr to approximately 10'4Torr.
13. A sample storage stage for an ultra-high vacuum instrument, comprising:a first sample parking position; a heating element adapted to apply heat to a sample loaded in the first sample parking position; one or more second sample parking positions; and a thermal insulating plate positioned to insulate the second sample parking positions from heat generated by the heating element.
14. The sample storage stage of claim 13, wherein the first and second sample parking positions are adapted to hold flag-type samples plates and the one or more second sample parking positions comprises four sample parking positions arranged in a stacked relationship.
15. The sample storage stage of any of claims 13-14, wherein the heating element comprises a filament through which electrical current flows.
16. The sample storage stage of any of claims 13-15, wherein the first sample parking position, heating element, thermal insulating plate, and second sample parking positions are arranged in a stacked relationship, and the thermal insulating plate is disposed between the heating element and the second sample parking positions.
17. The sample storage stage of any of claims 13-16, wherein the second sample parking positions are secured to a vacuum feedthrough flange by one or more first frames, and wherein the first sample parking position, heating element, and thermal insulating plate are secured to the second sample parking positions by one or more second frames.
18. The sample storage stage of any of claims 13-17, wherein the second sample parking positions are secured to a vacuum feedthrough flange by three first frames, and wherein the first sample parking position, heating element, and thermal insulating plate are secured to the second sample parking positions by three second frames.
19. The sample storage stage of any of claims 13-18, further comprising an electrical feedthrough for providing electrical current through the vacuum feedthrough flange to theheating element and for receiving a thermocouple temperature measurement signal from the heater.
20. A method of using the ultra-high vacuum instrument according to claim 1 to grow a film on a target sample comprising the steps of: cleaning the target sample surface with a sputtering gun; heating the target sample to flatten the surface; evaporating a target film material to enable growth of a target film on the target sample surface; and connecting at least one external vacuum system for additional sample processing.
21. The method of claim 20, further comprising the step of repeating the steps of cleaning and heating the target sample until an atomically flat sample surface is achieved.
22. A method of using the sample storage stage for an ultra-high vacuum instrument according to claim 13 comprising the steps of: loading a target sample in the first sample parking position; growing at least one target film on the target sample; and transferring the target sample to one of the second sample parking positions.
23. The method of claim 22, wherein the step of growing at least one target film comprises the steps of: cleaning the target sample surface with a sputtering gun; heating the target sample to flatten the surface; and evaporating a target film material to enable growth of a target film on the target sample surface.
24. The method of any of claims 22-23, further comprising the step of repeating the steps of loading, growing, and transferring for a plurality of target samples until each of the one or more second sample parking positions contains a target sample.
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