Deposition system for depositing a parylene film on a sample

Abstract

The present disclosure relates to a deposition system for depositing a parylene film on a sample. The deposition system includes a deposition chamber and a first vacuum pump subsystem. The deposition chamber includes a first flange interface configured as an access for transferring the sample to and from the deposition chamber, a second flange interface, a third flange interface, a sample holder disposed in the deposition chamber and configured to place the sample, a cylindrical cold trap disposed around the sample holder in the deposition chamber and provided with an opening on a side facing the first flange interface to allow the sample to pass through the opening to and from the sample holder, and a parylene cracking source mounted on the second flange interface of the deposition chamber facing the sample holder and configured to deposit a parylene film on the sample placed in the sample holder. The first vacuum pump subsystem is connected to the third flange interface of the deposition chamber and configured to provide a vacuum state of the deposition chamber.

Description

Technical Field

[0001] This disclosure relates to the field of optoelectronic devices, and more specifically, to a deposition system for depositing a parylene film on a sample. Background Technology

[0002] Various optoelectronic devices, such as perovskite optoelectronic devices and colloidal quantum dot optoelectronic devices, are receiving increasing attention from academia and industry due to their excellent properties. However, many optoelectronic devices, especially perovskite and colloidal quantum dot devices, are highly susceptible to corrosion from water and oxygen, leading to rapid performance degradation. To improve and stabilize the performance of optoelectronic devices, encapsulation is usually required. Summary of the Invention

[0003] According to a first aspect of this disclosure, a deposition system for depositing a parylene film on a sample is provided, comprising a deposition chamber and a first vacuum pump subsystem. The deposition chamber includes: a first flange interface, a second flange interface, and a third flange interface, the first flange interface being configured as an inlet / outlet for transferring a sample into and out of the deposition chamber; a sample holder disposed in the deposition chamber and configured to hold a sample; a cylindrical cold trap disposed in the deposition chamber surrounding the sample holder and having an opening on the side facing the first flange interface to allow the sample to pass through the opening into and out of the sample holder; and a parylene pyrolysis source mounted on the second flange interface of the deposition chamber facing the sample holder and configured to deposit a parylene film onto the sample placed in the sample holder. The first vacuum pump subsystem is connected to the third flange interface of the deposition chamber and configured to provide a vacuum state to the deposition chamber.

[0004] In some embodiments, the first flange interface is configured to connect to a fourth flange interface of a glove box in an inert gas atmosphere for preparing the sample, wherein the glove box is provided with a glove for operation on a first side and the fourth flange interface for connection to the deposition chamber of the deposition system on a second side, a first valve is installed at the fourth flange interface, the first valve allowing the sample to be transferred between the glove box and the deposition chamber when open, and isolating the glove box from the deposition chamber when closed, and the deposition system further includes: an inert gas source connected to the glove box and the deposition chamber, the inert gas source being configured to maintain the inert gas atmosphere of the glove box, and also being configured to be operable to achieve an inert gas atmosphere of the same or similar pressure as the glove box in the deposition chamber.

[0005] In some embodiments, the deposition system further includes: a pretreatment chamber connected between the fourth flange interface of the glove box and the first flange interface of the deposition chamber; a second valve mounted at the first flange interface, the second valve allowing the sample to be transferred between the pretreatment chamber and the deposition chamber when open, and isolating the pretreatment chamber from the deposition chamber when closed; and a second vacuum pump subsystem connected to the pretreatment chamber and configured to operate to achieve a vacuum state in the pretreatment chamber at the same or similar pressure as the deposition chamber, wherein the first valve allows the sample to be transferred between the glove box and the pretreatment chamber when open, and isolating the glove box from the pretreatment chamber when closed, and wherein the inert gas source is connected to the pretreatment chamber but not to the deposition chamber, and is configured to operate to achieve an inert gas atmosphere in the pretreatment chamber at the same or similar pressure as the glove box.

[0006] In some embodiments, the first vacuum pump subsystem includes a main pipeline section connected to the third flange interface, and a first branch pipeline section and a second branch pipeline section branching from the main pipeline section, and further includes a mechanical pump connected to the first branch pipeline section, a molecular pump connected to the second branch pipeline section, and a cold trap disposed around the main pipeline section, wherein the mechanical pump and the molecular pump are configured to operate to maintain the vacuum state of the deposition chamber at a vacuum state not greater than 0.1 Pa before the sample has been transferred to the sample holder and before the parylene pyrolysis source begins operation; and wherein the molecular pump is configured to be isolated from the deposition chamber during the operation of the parylene pyrolysis source.

[0007] In some embodiments, the sample holder further includes a cooling device configured to have thermal contact with the sample placed in the sample holder and to exchange heat with the cylindrical cold trap; wherein the cylindrical cold trap is a liquid nitrogen cold trap, and the projection of the cylindrical cold trap onto the plane of the parylene pyrolysis source covers the parylene pyrolysis source, and the parylene pyrolysis source extends into the cylindrical cold trap.

[0008] In some embodiments, the para-xylene pyrolysis source includes: a sublimation region comprising a crucible for containing para-xylene dimers and a first heating device for heating the para-xylene dimers to a sublimation temperature to cause sublimation; and a pyrolysis region configured to be closer to the sample holder than the sublimation region, and including a first conduit for causing sublimated para-xylene dimers received from the sublimation region to pyrolyze therein, wherein: the first conduit is configured to heat upon energization to heat the sublimated para-xylene dimers to a pyrolysis temperature to pyrolyze them into para-xylene monomers; and / or the pyrolysis region further includes a filament for emitting an electron beam into the first conduit. Furthermore, the first conduit is configured to heat up when bombarded by an electron beam to heat the sublimated p-xylene dimer to its pyrolysis temperature, thereby pyrolyzing it into p-xylene monomer; and / or the pyrolysis zone further includes a second heating device disposed within the first conduit, the second heating device being used to heat the sublimated p-xylene dimer to its pyrolysis temperature, thereby pyrolyzing it into p-xylene monomer; and / or the first conduit is thermally conductive, and the pyrolysis zone further includes a third heating device disposed outside the first conduit and in thermal contact with the first conduit, the third heating device being used to heat the sublimated p-xylene dimer to its pyrolysis temperature, thereby pyrolyzing it into p-xylene monomer.

[0009] In some embodiments, the par-xylene pyrolysis source further includes: a cooling zone configured to be closer to the sample holder than the pyrolysis zone, and including a second conduit for cooling the par-xylene monomer received from the pyrolysis zone therein, wherein the temperature of the cooling zone is set to be lower than the temperature at the pyrolysis zone and higher than the temperature at the sample holder.

[0010] In some embodiments, the second pipe is configured to exchange heat with a circulating water system, the temperature of which is controllable in order to control the temperature of the cooling zone.

[0011] In some embodiments, the deposition chamber further includes: a deposition rate measuring device configured to measure the parylene beam rate near the sample within the sample holder or the parylene film formation rate on the sample surface within the sample holder; and / or a baffle movable between a first position and a second position, wherein the baffle blocks the opening of the cylindrical cold trap when the baffle is in the first position, and does not block the opening of the cylindrical cold trap when the baffle is in the second position.

[0012] In some embodiments, the deposition chamber further includes a fifth flange interface configured to connect an additional deposition apparatus configured to deposit and grow organic, inorganic, and / or metallic materials.

[0013] Other features and advantages of this disclosure will become clearer from the following detailed description of exemplary embodiments with reference to the accompanying drawings. Attached Figure Description

[0014] The accompanying drawings, which form part of this specification, illustrate embodiments of this disclosure and, together with the specification, serve to explain the principles of this disclosure.

[0015] This disclosure will become clearer with reference to the accompanying drawings and the following detailed description, wherein: Figure 1 This is a top schematic block diagram of a deposition system for depositing a parylene film on a sample according to some embodiments of the present disclosure. Figure 2 This illustrates some embodiments according to the present disclosure. Figure 1 A side view schematic block diagram of an example structure of a sedimentation chamber in a sedimentation system; Figure 3 and Figure 4 These are examples illustrating some embodiments according to this disclosure. Figure 2 Side view and perspective view of an example structure of a cylindrical cold trap in a sedimentation chamber; Figure 5 This illustrates some embodiments according to the present disclosure. Figure 2 A three-dimensional view of an example structure of a sample holder in a deposition chamber; Figure 6 It is shown Figure 3 and Figure 4 The cylindrical cold trap and Figure 5 A three-dimensional view showing the sample holders assembled together; Figure 7 This is a schematic diagram illustrating the use of a deposition system in conjunction with a glove box according to some embodiments of the present disclosure; Figure 8 This is a schematic diagram illustrating the use of a deposition system in conjunction with a glove box according to other embodiments of the present disclosure; Figure 9 This illustrates some embodiments according to the present disclosure. Figure 1 A schematic block diagram of an example structure of the first vacuum pump subsystem in the system; Figure 10 This illustrates some embodiments according to the present disclosure. Figure 2 A side view of an example structure of a parylene pyrolysis source in a deposition chamber; Figure 11 This illustrates some embodiments according to the present disclosure. Figure 1 A schematic block diagram of another example structure of the deposition chamber in the system.

[0016] Note that in the embodiments described below, the same reference numerals are sometimes used across different figures to denote the same parts or parts having the same function, and repeated descriptions are omitted. In this specification, similar reference numerals and letters are used to denote similar items; therefore, once an item is defined in one figure, it does not need to be discussed further in subsequent figures.

[0017] For ease of understanding, the positions, dimensions, and extents of the structures shown in the accompanying drawings and other materials may not represent actual positions, dimensions, and extents. Therefore, the disclosed invention is not limited to the positions, dimensions, and extents disclosed in the accompanying drawings and other materials. Furthermore, the drawings are not necessarily drawn to scale, and some features may be enlarged to show details of specific components. Detailed Implementation

[0018] Various exemplary embodiments of the present disclosure will now be described in detail with reference to the accompanying drawings. It should be noted that, unless otherwise specifically stated, the relative arrangement, numerical expressions, and values ​​of the components and steps set forth in these embodiments do not limit the scope of the present disclosure.

[0019] The following description of at least one exemplary embodiment is merely illustrative and is in no way intended to limit this disclosure or its application or use. Those skilled in the art will understand that they merely illustrate exemplary ways that can be used to implement this disclosure, and are not exhaustive.

[0020] Techniques, methods, and equipment known to those skilled in the art may not be discussed in detail, but where appropriate, such techniques, methods, and equipment should be considered part of the specification.

[0021] Parylene (also known as para-xylene) is an excellent encapsulation material. It can be vapor-deposited onto prepared samples to form a conformal, low-light-loss thin film, effectively isolating the sample from external water and oxygen. Besides its use as an encapsulation material, an increasing number of optoelectronic devices are incorporating parylene films into their structures. Currently, parylene deposition requires a specialized vacuum deposition system. This system needs separate sublimation, pyrolysis, and deposition chambers to separately sublimate and pyrolyze the para-xylene dimer to obtain the para-xylene monomer, and then deposit and polymerize it to form a parylene film. Such specialized vacuum deposition systems for parylene are typically large and labor-intensive to operate. Because the adsorption rate of para-xylene monomer is too low above room temperature, during the deposition process, parylene films form not only on the sample surface but also at other locations within the vacuum deposition system. Over time, this can affect the operation of other functional components of the vacuum deposition system (e.g., vacuum pumps, valves). Therefore, it is necessary to frequently open the cavity of such a vacuum deposition system specifically designed for parylene to remove the parylene film on its inner surface.

[0022] Therefore, this disclosure provides a deposition system for depositing parylene films on samples. This system can achieve precise preparation of parylene films using a conventional single vacuum chamber combined with a parylene pyrolysis source specifically designed according to this disclosure. Furthermore, the entire system is robust, easy to maintain, and readily integrates with a glove box for in-situ encapsulation of parylene-based films. The deposition system for depositing parylene films on samples according to various embodiments of this disclosure will now be described in detail with reference to the accompanying drawings. It should be noted that actual deposition systems may include additional components, which will not be discussed herein and are not shown in the drawings to avoid obscuring the key points of this disclosure.

[0023] Figure 1 A deposition system 100 for depositing a parylene film on a sample is shown according to some embodiments of the present disclosure. Figure 1 As shown, system 100 includes a deposition chamber 120 and a first vacuum pump subsystem 130.

[0024] The deposition chamber 120 can be formed as any suitable vacuum cavity, such as a stainless steel cavity. (Refer to reference...) Figure 1 and Figure 2The deposition chamber 120 includes a first flange port 122, a second flange port 123, and a third flange port 124. The first flange port 122 is configured as an inlet / outlet for transferring samples into and out of the deposition chamber 120. The dimensions of the first flange port 122 can be designed to allow samples to pass through it, such as CF63, CF100, CF150, CF200, etc. It is understood that, here and elsewhere in this document, the flange specification is not limited to CF, and may also be other suitable flange specifications such as KF, ISO, etc. A first vacuum pump subsystem 130 is connected to the third flange port 124 of the deposition chamber 120 and is configured to provide a vacuum state for the deposition chamber 120. The deposition chamber 120 also includes a sample holder 121 disposed therein, which is configured to hold a sample. Figure 5 An example structure of sample holder 121 is shown schematically, but it is understood that sample holder 121 can be configured in any suitable form, without particular limitation.

[0025] The deposition chamber 120 also includes a cylindrical cold trap 126 disposed within the deposition chamber 120 surrounding a sample holder 121. The cylindrical cold trap 126 has an opening 1261 on the side facing the first flange interface 122 to allow a sample to pass through the opening 1261 into and out of the sample holder 121. The shape and size of the opening 1261 are not particularly limited, as long as it allows a sample to pass through, and a smaller opening 1261 is preferred. In some embodiments, the deposition chamber 120 may also include (e.g., via a lever) a baffle 1263 movable between a first position and a second position. When the baffle 1263 is in the first position, the baffle 1263 blocks the opening 1261 of the cylindrical cold trap 126, and when the baffle 1263 is in the second position, the baffle 1263 does not block the opening 1261 of the cylindrical cold trap 126. When the baffle 1263 is included, the opening 1261 is not necessarily smaller, as long as it allows a sample to pass through and is blocked by the baffle 1263. The presence of baffle 1263 allows for sample injection and effluent through opening 1261 without the risk of paraxylene dimer contaminating the cavity through opening 1261. Figure 3 and Figure 4 An example structure of the cylindrical cold trap 126 is shown. Figure 6 It shows Figure 5 Example sample holder 121 is set Figure 3 and Figure 4The example shown is a cylindrical cold trap 126. The cylindrical cold trap 126 is not limited to the cylindrical shape illustrated; it can also be other suitable shapes such as a square tube. In some embodiments, the cylindrical cold trap 126 can be a liquid nitrogen cold trap, which can receive liquid nitrogen, for example, from pipe 1262. In other embodiments, the cylindrical cold trap 126 can also be connected to an external refrigeration compressor. The cylindrical cold trap 126 can, for example, provide a temperature below room temperature, for example, not exceeding zero degrees Celsius, at or near the cylindrical cold trap 126. Temperature sensors (e.g., but not limited to thermocouples) can be placed at or near the cylindrical cold trap 126 to monitor its temperature.

[0026] The deposition chamber 120 also includes a parylene pyrolysis source 127, which is mounted on a second flange interface 123 of the deposition chamber 120 facing the sample holder 121 and configured to deposit a parylene film onto the sample placed in the sample holder 121. In some embodiments, the parylene pyrolysis source 127 is in the form of a k-cell evaporation beam source. The dimensions of the mounting flange 1274 of the parylene pyrolysis source 127 can be reasonably designed according to actual needs, for example, but not limited to, CF35, CF63, etc. In some embodiments, the deposition chamber 120 may also include a deposition rate measuring device (not shown), which can be configured to measure the parylene beam rate near the sample in the sample holder 121 (e.g., in the form of a crystal oscillator) or to measure the parylene film formation rate on the sample surface in the sample holder 121 (e.g., in the form of an in-situ ellipsometric film thickness gauge). Thus, precise control of the film thickness and deposition rate of the parylene sealing film can be achieved. It should be understood that the sample in the sample holder can be encapsulated using the parylene pyrolysis source 127, and / or a film layer can be deposited in the sample.

[0027] In some embodiments, the projection of the cylindrical cold trap 126 onto the plane containing the parylene pyrolysis source 127 covers the parylene pyrolysis source 127, and the parylene pyrolysis source 127 extends into the cylindrical cold trap 126. In some embodiments, the sample holder 121 may further include a cooling device 128 (e.g., but not limited to a copper block), which may be configured to have thermal contact with the sample placed in the sample holder 121 and to exchange heat with the cylindrical cold trap 126. A temperature detector (e.g., but not limited to a thermocouple) may be placed at or near the sample holder 121 to monitor its temperature.

[0028] Because the temperature of the cylindrical cold trap 126 is very low, even the lowest temperature in the deposition chamber 120, it is the place in the deposition chamber 120 where para-xylene monomers are most easily adsorbed to form a parylene film. Therefore, during the operation of the parylene pyrolysis source 127, para-xylene monomers are less likely to be ejected throughout the deposition chamber 120, thus preventing film deposition in undesirable areas such as the first vacuum pump system 130, and consequently reducing the risk of damage to the vacuum pump of the first vacuum pump system 130. This also makes the deposition chamber 120 easier to maintain.

[0029] In some embodiments, see, for example Figure 7 The first flange interface 122 of the deposition chamber 120 can be configured to connect to the fourth flange interface 112 of the glove box 110, which is in an inert gas atmosphere, for sample preparation. For example... Figure 7 As shown, the glove box 110 has an operating glove 111 on a first side 110A and a fourth flange interface 112 on a second side 110B for connection to the deposition chamber 120 of the deposition system 100. Although the first side 110A and the second side 110B are shown as opposite sides in the illustrated embodiment, this is merely exemplary and not limiting; the first side 110A and the second side 110B could also be adjacent sides or the same side, depending on the specific circumstances. A first valve 113 is installed at the fourth flange interface 112. When open, the first valve 113 allows sample transfer between the glove box 110 and the deposition chamber 120, and when closed, isolates the glove box 110 from the deposition chamber 120. The first valve 113 can be configured in any suitable form, such as being configured to rotate or translate relative to the first flange interface 112, without particular limitation. In such an embodiment, the deposition system 100 may further include an inert gas source 140 connected to the glove box 110 and the deposition chamber 120. The inert gas source 140 may be configured to maintain an inert gas atmosphere in the glove box 110 and is also configured to be operable to achieve an inert gas atmosphere in the deposition chamber 120 at the same or similar pressure as the glove box 110 (within a pressure difference range that allows the first valve 113 to be safely opened). As a non-limiting example, the inert gas source 140 may be a nitrogen source, and the glove box 110 may be a nitrogen glove box. The glove box 110 may be in an inert gas atmosphere and used for sample preparation therein.

[0030] Furthermore, the deposition chamber 120 of the deposition system 100 of this disclosure allows direct connection to the glove box 110, thereby facilitating in-situ (i.e., without exposure to the atmosphere) encapsulation of samples. For example, after isolating the first vacuum pump system 130 from the deposition chamber 120, the inert gas source 140 can be operated to create an inert gas atmosphere in the deposition chamber 120 with the same or similar pressure as the glove box 110 (within a pressure difference range that allows the first valve 113 to be safely opened). Then, the first valve 112 can be opened to transfer the sample prepared in the glove box 110 to the sample holder 121 in the deposition chamber 120. After the transfer is completed, the first valve 113 can be closed, and then the first vacuum pump system 130 can be operated to create an inert gas atmosphere in the deposition chamber. The desired vacuum state is achieved. Once this state is reached, the parylene pyrolysis source 127 is operated to deposit a parylene film on the sample. After deposition, the first vacuum pump system 130 is isolated from the deposition chamber 120, and the inert gas source 140 is operated to create an inert gas atmosphere in the deposition chamber 120 with the same or similar pressure as the glove box 110 (within a pressure difference range that allows the first valve 113 to be safely opened). Finally, the first valve 112 is opened to transfer the sample encapsulated in the deposition chamber 120 to the glove box 110. Thus, the sample is not exposed to the atmosphere throughout the entire process from preparation to encapsulation, resulting in excellent device performance.

[0031] Traditionally, no one has considered directly coupling a glove box to a dedicated vacuum deposition system for parylene. This is because, as mentioned earlier, the adsorption rate of parylene monomers is very low at temperatures above room temperature, making them prone to spreading during deposition. Therefore, if the glove box is directly coupled to the dedicated parylene vacuum deposition system, a parylene film will easily deposit inside the valve at the connection point. Over time, the valve will not be able to close completely, leading to leakage between the glove box and the vacuum deposition system. This will contaminate the glove box and compromise the vacuum level of the vacuum deposition system. Moreover, as mentioned earlier, maintenance of the dedicated parylene vacuum deposition system requires periodic opening to remove the parylene film from the inner walls. However, when the glove box is directly coupled to the parylene vacuum deposition system, it is inconvenient to enter the vacuum deposition system from the glove box for maintenance operations.

[0032] However, the inventors of this disclosure utilize a cylindrical cold trap 126 to bind the paraxylene monomers, which would otherwise easily wander around in the deposition chamber 120 after being pyrolyzed from the paraxylene pyrolysis source 127, to the cylindrical cold trap 126. This effectively prevents the paraxylene monomers from depositing as a film in other locations in the deposition chamber 120 besides the sample holder 121 containing the sample and the cylindrical cold trap 126. Consequently, it avoids damage to components such as the first valve 113 and the first vacuum pump subsystem 130 connected to the glove box 110 from paraxylene, and also eliminates the need to open the cavity to remove the paraxylene film from the inner wall.

[0033] In some embodiments, such as reference Figure 8 The deposition system 100 may further include a pretreatment chamber 150 and a second valve 151 mounted at a first flange interface 122. The pretreatment chamber 150 is connected between a fourth flange interface 112 of the glove box 110 and a first flange interface 122 of the deposition chamber 120. The second valve 151, when open, allows sample transfer between the pretreatment chamber 150 and the deposition chamber 120, and when closed, isolates the pretreatment chamber 150 from the deposition chamber 120. Additionally, the first valve 113, when open, allows sample transfer between the glove box 110 and the pretreatment chamber 150, and when closed, isolates the glove box 110 from the pretreatment chamber 150. The second valve 151 may take any suitable form, including but not limited to a slide gate valve. The deposition system 100 may further include a second vacuum pump subsystem 160 connected to the pretreatment chamber 150 and configured to operate such that the pretreatment chamber 150 achieves a vacuum state at the same or similar pressure as the deposition chamber 120 (within a pressure difference range that allows the second valve 151 to open safely). In some embodiments, the pretreatment chamber 150 may alternatively be evacuated using a first vacuum pump subsystem 130. An inert gas source 140 may be connected to the pretreatment chamber 150 but not to the deposition chamber 120 and is configured to operate such that the pretreatment chamber 150 achieves an inert gas atmosphere at the same or similar pressure as the glove box 110 (within a pressure difference range that allows the first valve 113 to open safely). The presence of the pretreatment chamber 150 allows the deposition chamber 120 to always be maintained in a better vacuum state without the need for repeated inert gas filling / evacuation. In addition, the volume of the pretreatment chamber 150 can be designed to be much smaller than that of the deposition chamber 120, thereby reducing the amount of gas used by the inert gas source 140.

[0034] In some embodiments, such as reference Figure 9The first vacuum pump subsystem 130 may include a main pipe section 138 connected to a third flange interface 124, and a first branch pipe section 136 and a second branch pipe section 137 branching off from the main pipe section 138. As a non-limiting example, the main pipe section 138, the first branch pipe section 136, and the second branch pipe section 137 may collectively form a tee. The first vacuum pump subsystem 130 may also include a mechanical pump 131 connected to the first branch pipe section 136, a molecular pump 132 connected to the second branch pipe section 137, and a cold trap 134 disposed around the main pipe section 138. The cold trap 134 is optional because the presence of the cylindrical cold trap 126 reduces the risk of poly(p-xylene) film deposition in the first vacuum pump subsystem 130. Of course, including the cold trap 134 may improve the effect. The cold trap 134 may be, for example, but is not limited to, a liquid nitrogen cold trap. It is also understood that the mechanical pump 131 can be replaced with another backing pump for rough vacuum, and the molecular pump 132 can be removed or replaced with another vacuum pump for high vacuum (e.g., a cryogenic pump). Valves 133, 135, etc., can also be provided to facilitate control of the first vacuum pump subsystem 130. In some embodiments, after the sample has been transferred to the sample holder 121 and before the parylene pyrolysis source 127 begins operation, the mechanical pump 131 and the molecular pump 132 can be configured to operate to maintain the vacuum state of the deposition chamber 120 at no more than 0.1 Pa or no more than 10 Pa. -2 Pa, or not greater than 10 -3 Pa, or not greater than 10 -4 Pa, or not greater than 10 -5 Pa, or not greater than 10 -6 Pa, or not greater than 10 - 7 Pa, or not greater than 10 -8 The vacuum state is Pa. At this time, valves 133 and 135 are both open. In some embodiments, during operation of the parylene pyrolysis source 127, the molecular pump 132 is configured to be isolated from the deposition chamber 120, for example by closing valve 135. At this time, valve 133 can remain open to maintain the vacuum state of the deposition chamber 120 by means of the mechanical pump 131.

[0035] In some embodiments, the par-xylene pyrolysis source 127 may include a sublimation region and a pyrolysis region. The sublimation region may include a crucible for containing par-xylene dimers and a first heating device for heating the par-xylene dimers to a sublimation temperature to cause sublimation. The pyrolysis region is positioned closer to the sample holder 121 than the sublimation region and includes a first conduit for causing the sublimated par-xylene dimers received from the sublimation region to pyrolyze therein. When the crucible is transparent to thermal radiation, such as a glass crucible, the first heating device may radiate heat to the par-xylene dimers in the crucible. When the crucible has a high thermal conductivity, such as a copper crucible, the first heating device may conduct heat to the par-xylene dimers in the crucible. In some examples, the first heating device is an electric heater that heats up when energized, such as a resistance wire wound around the crucible. In some examples, the first heating device may be a filament (e.g., but not limited to, a tungsten filament) for emitting an electron beam, and the material of the crucible (e.g., but not limited to, a tungsten crucible) may be configured to heat up when bombarded by an electron beam. In some examples, the first conduit may be configured to heat upon energization to raise the sublimated p-xylene dimer to its pyrolysis temperature, thereby pyrolyzing it into p-xylene monomers. In some examples, the pyrolysis zone may further include a filament (e.g., but not limited to, a tungsten filament) for emitting an electron beam into the first conduit, and the first conduit (e.g., but not limited to, a tungsten conduit) may be configured to heat upon being bombarded by the electron beam to raise the sublimated p-xylene dimer to its pyrolysis temperature, thereby pyrolyzing it into p-xylene monomers. In some examples, the pyrolysis zone may further include a second heating device disposed within the first conduit for raising the sublimated p-xylene dimer to its pyrolysis temperature, thereby pyrolyzing it into p-xylene monomers. In some examples, the second heating device is an electric heater that heats upon energization, such as a resistance wire wound within the first conduit. In some embodiments, the first conduit may be thermally conductive, and the pyrolysis zone may further include a third heating device disposed outside and in thermal contact with the first conduit for raising the sublimated p-xylene dimer to its pyrolysis temperature, thereby pyrolyzing it into p-xylene monomers. In some examples, the third heating device is an electric heater that heats up when energized, such as a resistance wire wound around the first conduit. In some embodiments, the parylene pyrolysis source 127 may also include a cooling zone positioned closer to the sample holder 121 than the pyrolysis zone, the cooling zone including a second conduit for cooling the parylene monomer received from the pyrolysis zone therein. The temperature of the cooling zone may be set below the temperature at the pyrolysis zone and above the temperature at the sample holder 121. In some examples, the second conduit may also be configured to exchange heat with a circulating water system, the temperature of which is controllable to control the temperature of the cooling zone.

[0036] Figure 10 A non-limiting example structure of parylene pyrolysis source 127 is shown. Figure 9As shown, the parylene pyrolysis source 127 includes a mounting flange 1274 for installation at a second flange interface 123 in the deposition chamber 120. The parylene pyrolysis source 127 also includes a sublimation zone 1271, a pyrolysis zone 1272, and a cooling zone 1273. The sublimation zone 1271 includes a crucible 12711 for containing parylene dimers and a first heating device 12712 for heating the parylene dimers to a sublimation temperature to induce sublimation. In some examples, a flange interface may be provided at the end of the sublimation zone 1271 to allow for the installation and removal of the crucible 12711 for maintenance operations such as packing and cleaning. The pyrolysis zone 1272 includes a first conduit 12721 and a second heating device 12722 disposed within the first conduit 12721. The first conduit 12721 receives sublimated p-xylene dimers from the sublimation zone 1271, and the second heating device 12722 heats the sublimated p-xylene dimers to the pyrolysis temperature, thereby pyrolyzing them into p-xylene monomers. This internal heating method can efficiently utilize the heat generated by the second heating device 12722. The cooling zone 1273 may include a second conduit 12731, and a circulating water system (not shown) can supply and recover circulating water to and from the second conduit 12731 via an interface 12732. The parylene pyrolysis source 127 also includes an electrical feedthrough 1275 for supplying power to components within the parylene pyrolysis source 127 and for collecting temperature sensing signals from it when one or more temperature detectors (e.g., but not limited to thermocouples) are disposed within the parylene pyrolysis source 127. In the illustrated embodiment, the longitudinal axis of the sublimation region 1271 is set to be orthogonal to the longitudinal axes of the pyrolysis region 1272 and the cooling region 1273 in order to save space, but this is merely exemplary and not limiting. The longitudinal axis of the sublimation region 1271 may also be set to coincide with the longitudinal axes of the pyrolysis region 1272 and the cooling region 1273. Additionally, in the illustrated embodiment, the sublimation zone 1271 is illustrated below the mounting flange 1274 (i.e., all of it will be located outside the deposition chamber 120), the pyrolysis zone 1272 is illustrated across the mounting flange 1274 (i.e., part of it will be located outside the deposition chamber 120 and another part will be located inside the deposition chamber 120), and the cooling zone 1273 is illustrated above the mounting flange 1274 (i.e., all of it will be located inside the deposition chamber 120). However, this is merely exemplary and not limiting. For example, the sublimation zone 1271, the pyrolysis zone 1272, and the cooling zone 1273 could all be located above the mounting flange 1274 (i.e., the sublimation zone 1271, the pyrolysis zone 1272, and the cooling zone 1273 would all be located inside the deposition chamber 120).

[0037] In some embodiments, the deposition chamber 120 may further include one or more fifth flange interfaces, which may be configured to connect additional deposition devices. The additional deposition devices may be separate growth sources (e.g., tungsten boats, k-cell beam sources, etc.) or other deposition systems (e.g., molecular beam epitaxy cavities, electron beam sputtering cavities, vacuum thermal evaporation cavities, etc.). The additional deposition devices may be configured to deposit organic, inorganic, and / or metallic materials. In this way, the deposition chamber 120 can not only be used to encapsulate samples with parylene or form parylene films in samples, but also participate in the preparation of other films on the sample, such as for depositing organic small molecule electron / hole transport materials, metallic electrode materials, etc.

[0038] For example, in Figure 11 In the illustrated embodiment, the deposition chamber 120 further includes a fifth flange interface 125 on which a growth source 128 is mounted. Although in the illustrated embodiment, the growth source 128 also extends into the cylindrical cold trap 126, this is merely exemplary and not limiting. As a non-limiting example, when the sample is a colloidal quantum dot laser, the growth source 128 can, for example, be used to grow a dielectric material (e.g., molybdenum oxide or lithium fluoride) with a different dielectric constant (preferably a large difference) than parylene, thereby enabling it to cooperate with the parylene pyrolysis source 127 to form a distributed Bragg reflector (DBR) structure for the colloidal quantum dot laser. Taking a lithium fluoride k-cell beam source as an example, a top DBR structure with multiple pairs of parylene and lithium fluoride film layers stacked together can be fabricated using the parylene pyrolysis source 127 and the lithium fluoride k-cell beam source 128, thus serving as a top reflector for the colloidal quantum dot laser. In each pair of parylene and lithium fluoride layers, the thicknesses of the parylene and lithium fluoride layers can be the same or different, and can range from, for example, 1 nanometer to 1000 nanometers, depending on the resonant wavelength of the colloidal quantum dot laser. Such a DBR structure can, for example, include a periodic structure of several to dozens of pairs of parylene and lithium fluoride layers. The layer in the top DBR structure closest to the colloidal quantum dot laser can be the parylene layer, thus encapsulating the underlying laser. An additional parylene layer can also be formed on top of the top DBR structure to encapsulate the underlying lithium fluoride layer and prevent it from being affected by water and oxygen.

[0039] The terms “left,” “right,” “front,” “back,” “top,” “bottom,” “upper,” “lower,” “high,” “lower,” etc., used in the specification and claims, if present, are for descriptive purposes and not necessarily for describing constant relative positions. It should be understood that such terms are interchangeable where appropriate, so that embodiments of this disclosure described herein can operate, for example, in orientations different from those shown or otherwise described herein. For example, when the device in the drawings is reversed, a feature previously described as “above” other features may now be described as “below” other features. The device may also be oriented in other ways (rotated 90 degrees or in other orientations), in which case the relative spatial relationships will be interpreted accordingly.

[0040] In the specification and claims, when an element is described as being "on top of," "attached to," "connected to," "coupled to," or "in contact with" another element, the element may be directly located on top of, directly attached to, directly connected to, directly coupled to, or directly in contact with the other element, or one or more intermediate elements may be present. Conversely, when an element is described as being "directly" located on top of, directly attached to, directly connected to, directly coupled to, or directly in contact with another element, no intermediate elements are present. In the specification and claims, when a feature is arranged "adjacent" to another feature, it may mean that a feature has a portion overlapping with the adjacent feature or a portion located above or below the adjacent feature.

[0041] As used herein, the term "exemplary" means "serving as an example, instance, or illustration," and not as a "model" to be precisely copied. Any implementation described herein by example is not necessarily to be construed as preferred or advantageous over other implementations. Furthermore, this disclosure is not limited to any theory expressed or implied as given in the art, background, summary of the invention, or detailed description.

[0042] As used herein, the term "substantially" means any minor variation resulting from design or manufacturing defects, device or component tolerances, environmental influences, and / or other factors. The term "substantially" also allows for differences from the perfect or ideal situation due to parasitic effects, noise, and other practical considerations that may exist in the actual implementation.

[0043] Additionally, terms such as “first,” “second,” etc., may be used in this document for reference purposes only and are not intended to be limiting. For example, unless the context clearly indicates otherwise, the words “first,” “second,” and other such numerical terms relating to structures or elements do not imply order or sequence.

[0044] It should also be understood that when the term “including / contains” is used herein, it indicates the presence of the indicated feature, whole, step, operation, unit and / or component, but does not preclude the presence or addition of one or more other features, wholes, steps, operations, units and / or components and / or combinations thereof.

[0045] In this disclosure, the term “provide” is used broadly to cover all ways of obtaining an object, and therefore “provide an object” includes, but is not limited to, “purchasing,” “preparing / manufacturing,” “arranging / setting up,” “installing / assembling,” and / or “ordering” an object.

[0046] As used herein, the term “and / or” includes any and all combinations of one or more of the listed items in association. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of this disclosure. As used herein, the singular forms “a,” “an,” and “the” are also intended to include the plural forms unless the context clearly indicates otherwise.

[0047] Those skilled in the art will recognize that the boundaries between the above operations are merely illustrative. Multiple operations may be combined into a single operation, a single operation may be distributed among additional operations, and operations may be performed with at least partial overlap in time. Moreover, alternative embodiments may include multiple instances of a particular operation, and the order of operations may be changed in various other embodiments. However, other modifications, variations, and substitutions are equally possible. Aspects and elements of all the embodiments disclosed above may be combined in any way and / or in combination with aspects or elements of other embodiments to provide multiple additional embodiments. Therefore, this specification and the accompanying drawings should be considered illustrative rather than restrictive.

[0048] While specific embodiments of this disclosure have been described in detail by way of example, those skilled in the art should understand that the examples are for illustrative purposes only and not intended to limit the scope of this disclosure. The various embodiments disclosed herein can be combined in any way without departing from the spirit and scope of this disclosure. Those skilled in the art should also understand that various modifications can be made to the embodiments without departing from the scope and spirit of this disclosure. The scope of this disclosure is defined by the appended claims.

Claims

1. A deposition system for depositing a parylene film on a sample, comprising: The sedimentation chamber includes: The system includes a first flange interface, a second flange interface, and a third flange interface, wherein the first flange interface is configured as an inlet / outlet for transferring samples into and out of the deposition chamber. A sample holder, disposed in the deposition chamber and configured to hold a sample. A cylindrical cold trap is arranged around the sample holder in the deposition chamber, and has an opening on the side facing the first flange interface to allow the sample to pass through the opening into and out of the sample holder. A parylene pyrolysis source is mounted on the second flange interface of the deposition chamber facing the sample holder and configured to deposit a parylene film onto the sample placed in the sample holder; and A first vacuum pump subsystem, connected to the third flange interface of the deposition chamber and configured to provide a vacuum state for the deposition chamber, The cylindrical cold trap is a liquid nitrogen cold trap, and the projection of the cylindrical cold trap on the plane where the parylene pyrolysis source is located covers the parylene pyrolysis source, and the parylene pyrolysis source extends into the cylindrical cold trap.

2. The deposition system according to claim 1, wherein, The first flange interface is configured to connect to a fourth flange interface of a glove box in an inert gas atmosphere for preparing the sample, wherein the glove box has a glove provided on a first side for operation and a fourth flange interface provided on a second side for connection to the deposition chamber of the deposition system. A first valve is installed at the fourth flange interface, which, when open, allows the transfer of the sample between the glove box and the deposition chamber, and when closed, isolates the glove box from the deposition chamber. The deposition system further includes: An inert gas source is connected to the glove box and the deposition chamber, the inert gas source being configured to maintain the inert gas atmosphere in the glove box and also being operable to achieve an inert gas atmosphere in the deposition chamber at the same or similar pressure as the glove box.

3. The deposition system according to claim 2, further comprising: A pretreatment chamber is connected between the fourth flange interface of the glove box and the first flange interface of the deposition chamber; A second valve is installed at the first flange interface, which, when open, allows the sample to be transferred between the pretreatment chamber and the deposition chamber, and when closed, isolates the pretreatment chamber from the deposition chamber; A second vacuum pump subsystem is connected to the pretreatment chamber and configured to operate such that the pretreatment chamber achieves a vacuum state with the same or similar pressure as the deposition chamber. The first valve, when open, allows the sample to be transferred between the glove box and the pretreatment chamber, and when closed, isolates the glove box from the pretreatment chamber. The inert gas source is connected to the pretreatment chamber but not to the deposition chamber, and is configured to operate such that the pretreatment chamber has an inert gas atmosphere at the same or similar pressure as the glove box.

4. The deposition system according to claim 1, wherein, The first vacuum pump subsystem includes a main pipeline section connected to the third flange interface, a first branch pipeline section and a second branch pipeline section branching off from the main pipeline section, and further includes a mechanical pump connected to the first branch pipeline section, a molecular pump connected to the second branch pipeline section, and a cold trap disposed around the main pipeline section. Specifically, before the sample has been transferred to the sample holder and before the parylene pyrolysis source begins operation, the mechanical pump and molecular pump are configured to operate to maintain the vacuum state of the deposition chamber at a vacuum state not exceeding 0.1 Pa; and During the operation of the parylene cracking source, the molecular pump is configured to be isolated from the deposition chamber.

5. The deposition system according to claim 1, in, The sample holder also includes a cooling device configured to have thermal contact with the sample placed in the sample holder and to exchange heat with the cylindrical cold trap.

6. The deposition system according to claim 1, wherein, The parylene pyrolysis source includes: The sublimation zone includes a crucible for containing the p-xylene dimer and a first heating device for heating the p-xylene dimer to a sublimation temperature to cause sublimation. A pyrolysis zone, configured to be closer to the sample holder than the sublimation zone, includes a first conduit for causing the sublimated p-xylene dimer received from the sublimation zone to pyrolyze therein, wherein: The first conduit is configured to heat upon energization to raise the sublimated p-xylene dimer to its pyrolysis temperature, thereby pyrolyzing it into p-xylene monomer; and / or The pyrolysis zone further includes a filament for emitting an electron beam into the first conduit, and the first conduit is configured to heat up when bombarded by the electron beam to heat the sublimated p-xylene dimer to the pyrolysis temperature, thereby pyrolyzing it into p-xylene monomers; and / or The pyrolysis zone further includes a second heating device disposed within the first pipe, the second heating device being used to heat the sublimated p-xylene dimer to the pyrolysis temperature to pyrolyze it into p-xylene monomer; and / or The first pipe is thermally conductive, and the pyrolysis zone further includes a third heating device disposed outside the first pipe and in thermal contact with the first pipe, the third heating device being used to heat the sublimated p-xylene dimer to the pyrolysis temperature to pyrolyze it into p-xylene monomer.

7. The deposition system according to claim 6, wherein, The par-xylene pyrolysis source also includes: A cooling zone is configured to be closer to the sample holder than the pyrolysis zone and includes a second conduit for cooling the paraxylene monomer received from the pyrolysis zone therein, wherein the temperature of the cooling zone is set to be lower than the temperature at the pyrolysis zone and higher than the temperature at the sample holder.

8. The deposition system according to claim 7, wherein, The second pipe is configured to exchange heat with a circulating water system, the temperature of which is controllable in order to control the temperature of the cooling zone.

9. The deposition system according to claim 1, wherein, The deposition chamber also includes: A deposition rate measuring device is configured to measure the parylene beam rate near the sample within the sample holder or the parylene film formation rate on the surface of the sample within the sample holder; and / or A baffle movable between a first position and a second position, wherein the baffle blocks the opening of the cylindrical cold trap when the baffle is in the first position, and does not block the opening of the cylindrical cold trap when the baffle is in the second position.

10. The deposition system according to claim 1, wherein, The deposition chamber also includes a fifth flange interface configured to connect an additional deposition device configured to deposit and grow organic, inorganic, and / or metallic materials.

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