Vacuum coating material mass production performance evaluation device

Abstract

Disclosed is a vacuum coating material mass production performance evaluation device. The device comprises at least one vertically arranged material container, at least one vacuum device and at least one heating device; the material container is tubular and comprises a part A and a part B, the part B is used for containing the material to be tested and ensuring a certain longitudinal accumulation; the part A is used for collecting the sublimation deposited material, and the connection between the part A and the part B has a diameter change, which can effectively avoid the material deposited in the part A from falling and damaging the ash layer of the part B. A small amount of material can be used to simulate the performance of a large amount of vacuum coating material continuously evaporated at a high temperature on a mass production line, so that the mass production performance of the vacuum coating material can be simply, intuitively and effectively evaluated, and the adverse effects or losses on production can be avoided.

Description

Technical Field

[0001] This invention relates to an evaluation device for vacuum-coated materials, and more particularly, to a mass production performance evaluation device for vacuum-coated materials. Background Technology

[0002] A key step in OLED panel manufacturing is vacuum thermal evaporation of OLED materials. This process is completed using an evaporation machine under high vacuum and high temperature conditions. During this process, if material needs to be replenished, the temperature must be lowered and the vacuum broken. After replenishment, the vacuum level must be restored to the required operating temperature, which takes a considerable amount of time (usually around 48 hours). Therefore, to improve machine utilization, the common practice is to load a sufficient amount of material into the evaporation machine at once (typically large quantities, such as hundreds of grams of luminescent dopant and several kilograms or more of the main material) to meet the needs of long-term continuous evaporation. Currently, a typical warehousing cycle in the industry is 7-14 days. Within this cycle, the material is generally maintained at a relatively high temperature for continuous evaporation production, thus requiring high thermal stability of the candidate OLED mass-production materials. Candidate OLED mass-production materials may decompose and generate ash during prolonged high-temperature evaporation on the production line. (Although the industry's understanding of the formation mechanism and composition of ash is not yet clear, it is generally believed that ash is a complex mixture produced after the decomposition of OLED materials. Its evaporation temperature is much higher than that of the OLED materials, and it covers the surface of the material to be evaporated, affecting the evaporation rate and temperature.) Ash covering the surface of the material to be evaporated reduces the evaporation rate. To maintain the required evaporation rate for production, the evaporation temperature needs to be further increased, which in turn exacerbates the decomposition of the remaining material to be evaporated, leading to a vicious cycle. In severe cases, the decomposition of OLED materials can reduce the quality of the produced OLED panels, resulting in significant economic losses.

[0003] To avoid such serious problems on the production line, it is crucial to evaluate the mass production performance (thermal stability) of OLED materials or other vacuum-coated materials before mass production. Currently, there are three main methods.

[0004] Method one is the most direct evaluation method: on a mass production vapor deposition machine, vapor deposition and baking are performed according to the material usage, vapor deposition rate (corresponding to vapor deposition temperature), and vapor deposition time in actual mass production. Although this method is the most realistic and reliable, it consumes a significant amount of machine time on the mass production equipment and wastes a large amount of expensive vacuum coating material (such as tens to hundreds of grams for luminescent doped materials). Furthermore, if the material undergoes severe decomposition during the verification process, generating a large amount of ash, it may contaminate the mass production line, causing further economic losses. Therefore, the usual practice is to schedule such an evaluation only after the candidate mass production material has passed R&D verification and entered the pilot production stage. Clearly, before this, the good thermal stability of the candidate mass production material has already been confirmed through other methods.

[0005] Method two, commonly used in the industry to assess the thermal stability of materials, is the ampoule test, an indirect testing method. A small amount of material is placed in a glass test tube, which is then evacuated and its opening sintered and sealed. The test tube containing the vacuum-coated material is then placed in a tubular heating device and heated continuously at high temperature for a certain period (e.g., 7 days). This method is also known as the sealed-tube aging test. This method judges the thermal stability of the material by comparing its properties, purity, and device performance before and after the experiment, thus indirectly evaluating the mass production performance of vacuum-coated materials. In this aging test, because the glass test tube containing the vacuum-coated material is sealed, substances generated under high-temperature conditions cannot be removed by the vacuuming process. Even if ash is generated, it adheres to the molecular surface, making it impossible to directly assess the ash generation. Simultaneously, the entire sealed tube is in a high-temperature region without temperature changes, preventing the material from undergoing sublimation and redeposition, which differs significantly from the actual mass production vapor deposition process. Obviously, although this method uses a small amount of material, it cannot intuitively judge the changes in the material, nor can it effectively simulate the aging process of vacuum-deposited materials in an evaporation machine.

[0006] Method three utilizes existing sublimation apparatuses for purifying vacuum-deposited materials: the vacuum-deposited material to be tested is sublimated for an extended period (e.g., 7 days), and the changes in material properties and ash production before and after sublimation are observed. Mass production performance is evaluated primarily by comparing the purity and device performance before and after sublimation. While this method more directly and realistically simulates the high-temperature, high-vacuum environment of mass production compared to Method two, it, like Method two, still relies mainly on comparing test data before and after sublimation, making it a relatively indirect method. Furthermore, the primary design purpose of such sublimation purification equipment is to rapidly sublimate and purify large quantities of vacuum-deposited materials, typically by spreading the material evenly in a sublimation boat. Even if ash is produced, it will be a thin layer, difficult to observe, and difficult to completely extract for physicochemical analysis. Additionally, the diameter of the sublimation tube in the apparatus is generally greater than 30 mm, requiring a relatively large amount of material.

[0007] CN207169087U discloses an organic material sublimation purification apparatus. The container holding the material to be sublimated is placed horizontally. Its purpose is to sublimate and purify the material, not to assess its thermal stability. During the sublimation process, even if ash is generated, it only forms a very thin layer, which is inconvenient to measure and record, making it difficult to assess the material's thermal stability. US7,611,548 B2 describes a vertical sublimation apparatus used to sublimate and purify organic materials. Its material container is also placed horizontally in a heating zone, but the area where the material sublimates and deposits is set as a vertical channel. Therefore, it suffers from a similar problem to CN207169087U: it is not used to assess the material's thermal stability, and even if ash is generated, it is difficult to observe and test, thus making it difficult to assess the material's thermal stability.

[0008] Therefore, developing equipment and methods for assessing the thermal stability of materials with minimal material consumption and in a simpler and more intuitive way is of great practical significance for evaluating the mass production performance of materials. Summary of the Invention

[0009] This invention aims to provide a device for evaluating the mass production performance of vacuum-deposited materials to solve at least some of the aforementioned problems. The device employs a vertically arranged, tubular material container comprising two parts: Part A and Part B. Part B holds the material to be tested, ensuring a certain vertical accumulation within a high-temperature zone. Part A, located in a low-temperature zone, collects the sublimated material. A change in diameter at the junction of Part A and Part B effectively prevents material deposited in Part A from falling off and damaging the ash layer in Part B. This device can simulate the performance of large quantities of vacuum-deposited materials continuously deposited at high temperatures on a mass production line using only a small amount of material. It provides a simple, intuitive, and effective evaluation of the mass production performance of vacuum-deposited materials, avoiding adverse effects or losses on production.

[0010] According to an embodiment of the present invention, a vacuum coating material mass production performance evaluation device is disclosed, which includes: at least one material container, at least one vacuum device and at least one heating device;

[0011] The material container is tubular and comprises at least part A and part B; part A has a diameter D. A One end of part B is closed, and the portion of part B furthest from the closed end has a diameter D. b And D b Less than D A The other end of part B is connected to part A; one end of part A away from the connection between part A and part B is connected to the at least one set of vacuum devices; the material container is in a vertical position; and A is located above B.

[0012] The heating device includes at least one heating cavity C, the heating cavity C having a diameter D. C It can accommodate vertically placed material containers.

[0013] In this embodiment, because the portion of part B furthest from the closed end has a diameter D b And D b Less than D A This special structural design allows for a change in diameter at the connection between parts A and B, forming a platform-like or trough-like region. After the material in part B sublimates and deposits in part A, under the influence of gravity or mechanical vibration, material particles falling from part A will land in the platform-like or trough-like region, rather than in part B, thus avoiding disruption of any potential ash stratification. It is clearly understood that the D... b It can be a single value or a series of varying values, when D b When it is a series of changing values, at least one of them, D, must be a D. b Less than D A .

[0014] In this embodiment, the heating chamber C includes at least one high-temperature zone and at least one low-temperature zone, with the low-temperature zone above the high-temperature zone. In operation, portion B of the material container is located in the high-temperature zone, and portion A is located in the low-temperature zone, creating a temperature gradient between portion A and portion B. Material placed in portion B can cool and deposit in portion A after evaporation / sublimation.

[0015] According to one embodiment of the present invention, the portion of part B that is away from the connection between part A and part B is the main body portion, and the main body portion has a diameter D. B And D A / D B ≥ 1.

[0016] According to one embodiment of the present invention, the portion of part B that is away from the connection between part A and part B is the main body portion, and the main body portion has a diameter D. B And D A / D B ≥ 1, D B / D b ≥ 1.

[0017] According to one embodiment of the present invention, one end of the B portion that connects to the A portion protrudes a certain distance into the interior of the A portion to form a barrier.

[0018] According to one embodiment of the present invention, the B portion has a uniform diameter, or the end of the B portion connected to the A portion has a change in diameter, for example, expanding from bottom to top and then narrowing to protrude into the interior of the A portion, or narrowing directly from bottom to top to protrude into the interior of the A portion.

[0019] According to one embodiment of the present invention, the diameter of the end of the B portion connected to the A portion has various variations, for example, it gradually changes from bottom to top, first narrowing to form a narrow channel, then widening to match the connection with the A portion, and then narrowing again to protrude into the interior of the A portion.

[0020] According to one embodiment of the present invention, the A portion and the B portion have a concentric axis.

[0021] According to one embodiment of the present invention, wherein the D A / D B Greater than or equal to 1.

[0022] According to one embodiment of the present invention, wherein the D A / D B Greater than or equal to 1.5.

[0023] According to one embodiment of the present invention, wherein the D A / D B Greater than or equal to 1.7.

[0024] According to one embodiment of the present invention, wherein the D A / D B Greater than or equal to 2.

[0025] According to one embodiment of the present invention, wherein the D A / D B Greater than or equal to 2.5.

[0026] According to one embodiment of the present invention, wherein the D A / D B ≤3.

[0027] According to one embodiment of the present invention, wherein the D B ≤30 mm.

[0028] According to one embodiment of the present invention, wherein the D B ≤20 mm.

[0029] According to one embodiment of the present invention, wherein the D B ≤10 mm.

[0030] According to one embodiment of the present invention, the A portion and the B portion are integrally connected without being detached.

[0031] According to one embodiment of the present invention, the A portion and the B portion are detachably connected as a single unit.

[0032] According to one embodiment of the present invention, the bottom of part B is a curved surface or a flat surface.

[0033] According to one embodiment of the present invention, the length of part B is ≤100 mm, and the length of part A is greater than or equal to the length of part B.

[0034] According to one embodiment of the present invention, the material container has graduations on its tube wall.

[0035] According to one embodiment of the present invention, the tube wall of section B is provided with graduations.

[0036] According to one embodiment of the present invention, the material of the material container is a transparent material.

[0037] According to one embodiment of the present invention, the material of the material container is quartz or glass.

[0038] According to one embodiment of the present invention, the vacuum device includes a vacuum apparatus and a vacuum line connecting the material container and the vacuum apparatus.

[0039] According to one embodiment of the present invention, the vacuum equipment includes a mechanical pump and a molecular pump, and the vacuum pipeline is provided with a valve and a vacuum degree measuring device.

[0040] According to one embodiment of the present invention, the vacuum measuring device includes a vacuum gauge and related supporting display devices.

[0041] According to one embodiment of the present invention, the vacuum degree measuring device has a vacuum degree measuring range of 1.0*10. -6 Pa-1.0*10 5 Pa.

[0042] According to one embodiment of the present invention, the heating device can heat to a maximum temperature of 1000 °C.

[0043] According to one embodiment of the present invention, the heating cavity of the heating device is a cylindrical cavity with a diameter D. C .

[0044] In this embodiment, the diameter D of the heating chamber is [specified] in order to accommodate the material container. C >D A Preferably, in order to facilitate better heat transfer from the heating chamber to the material container and reduce the temperature difference between the heating chamber wall and the material container, D A With D C The difference shouldn't be too large, generally D A ≥Dc-100 mm; preferably, D C >D A ≥D C -10 mm; more preferably, D C >D A ≥D C -5 mm; most preferably, D C >D A ≥D C -3 mm.

[0045] According to one embodiment of the present invention, the heating cavity of the heating device includes at least a portion C1 and a portion C2, with portion C1 located above portion C2 and having a diameter D respectively. C1 and D C2 And satisfy the following conditions: D C1 >D A ≥D C1 -100mm, D C2 >D B ≥DC2 -100 mm; preferably, D C1 >D A ≥D C1 -10 mm, D C2 >D B ≥D C2 -10 mm; more preferably, D C1 >D A ≥D C1 -5 mm, D C2 >D B ≥D C2 -5 mm; most preferably, D C1 >D A ≥D C1 -3 mm, D C2 >D B ≥D C2 -3 mm.

[0046] According to one embodiment of the present invention, the heating device includes at least two temperature zones, a and b, where a is located above b, and the temperatures of a and b can be controlled independently.

[0047] According to one embodiment of the present invention, the at least one heating device includes a plurality of heating chambers, each of which independently has the same or different shapes and sizes.

[0048] According to one embodiment of the present invention, the device further includes a plurality of heating devices, each heating device having at least two temperature zones, and each temperature zone having independently controllable temperature; the plurality of heating devices are coupled with a vacuum device.

[0049] According to one embodiment of the present invention, the heating device further includes a lifting device and / or an observation window.

[0050] According to another embodiment of the present invention, a method for evaluating the mass production performance of vacuum-deposited materials using the vacuum-deposited material mass production performance evaluation apparatus as shown in any of the above embodiments is disclosed, comprising the following steps:

[0051] Step 1: Obtain the material to be tested.

[0052] Step two: Fill the material to be tested into the material container and record the relevant information.

[0053] Step 3: Install the material container in place.

[0054] Step four, vacuum extraction.

[0055] Step 5: Heat to a certain temperature and continue baking for a certain period of time.

[0056] Step six: Record the data.

[0057] According to one embodiment of the present invention, the method further includes the step of determining a heating temperature T, wherein the heating temperature T is determined according to any of the following methods:

[0058] (1) The heating temperature T is the vapor deposition temperature of the material to be tested on the mass production vapor deposition machine or the average value of the vapor deposition temperature;

[0059] (2) The heating temperature T is the vapor deposition temperature of the material to be tested on the vapor deposition machine plus a certain temperature ΔT;

[0060] Wherein, ΔT ≤ 75 ℃;

[0061] The aforementioned steps can occur before step five.

[0062] According to one embodiment of the present invention, the method further includes the step of determining a baking time t, wherein the baking time t is determined according to any of the following methods:

[0063] (1) The baking time t is 7 days, 10 days or 14 days;

[0064] (2) The baking time t is the time when the material to be tested exhibits ash or abnormalities during sublimation on the mass production performance evaluation device;

[0065] The aforementioned steps can occur before step five.

[0066] According to one embodiment of the present invention, the method further includes measuring the physical properties of the material to be tested before and after the experiment, the physical properties including but not limited to purity, melting point, glass transition temperature, and decomposition temperature.

[0067] According to one embodiment of the present invention, the data recording step further includes measuring and recording the height of the ash content.

[0068] According to one embodiment of the present invention, the data recording step further includes measuring and recording the physical properties of ash, including but not limited to purity, melting point, glass transition temperature, and decomposition temperature.

[0069] According to one embodiment of the present invention, the data recording step further includes calculating the average sublimation rate v.

[0070] According to one embodiment of the present invention, the device test results of the material under test are further recorded in the data recording step.

[0071] According to another embodiment of the present invention, the use of the aforementioned vacuum coating material mass production performance evaluation device as a micro-material sublimation device is also disclosed.

[0072] This invention discloses a vacuum coating material mass production performance evaluation device. The material container is vertically arranged and comprises two parts, A and B. Part B holds the material to be tested, ensuring a certain vertical accumulation within the container, and is located in a high-temperature zone. Part A, located in a low-temperature zone, collects the sublimated material. This device can simulate the performance of continuous high-temperature evaporation of large quantities of vacuum coating material on a mass production line using only a small amount of material. It provides a simple, intuitive, and effective evaluation of the mass production performance of vacuum coating materials, avoiding adverse effects or losses on production. Furthermore, this device can also be used as a micro-sublimation device, saving equipment costs and space, making it convenient and efficient. Attached Figure Description

[0073] Fig. 1a This is a schematic diagram of the structure of a vacuum coating material mass production performance evaluation device according to the present invention; Fig. 1b This is a schematic diagram of the structure of a vacuum device according to the present invention; Fig. 1c-Fig. 1d This is a schematic diagram of the heating device of the present invention.

[0074] Fig. 2a-2e This is a schematic diagram of the material container of the present invention.

[0075] Fig. 3 This is a schematic diagram of an openable heating device according to the present invention.

[0076] Fig. 4 This is a schematic diagram of another vacuum coating material mass production performance evaluation device according to the present invention.

[0077] Fig. 5 This is a schematic diagram of another vacuum coating material mass production performance evaluation device according to the present invention.

[0078] Fig. 6 This is a flowchart of a method for evaluating the mass production performance of vacuum coating materials according to the present invention. Detailed Implementation

[0079] To make the technical problems solved by the present invention, the technical solutions adopted, and the technical effects achieved clearer, the technical solutions of the present invention will be further described below in conjunction with the accompanying drawings and specific embodiments.

[0080] In this article, vacuum coating materials refer to materials that can be deposited in a vacuum through vacuum thermal evaporation to form a film, including organic materials, metallic materials, oxides, and other materials that can be used to prepare organic electronic devices through vacuum thermal evaporation.

[0081] In the description of this invention, the terms "vertical," "horizontal," etc., indicate that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. "Horizontal" refers to being on a horizontal plane in real space, and "vertical" refers to being perpendicular to a horizontal plane in real space.

[0082] In the description of this invention, it should be understood that the terms "center," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," and "circumferential" indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are used only for the convenience of describing this invention and simplifying the description, and are not intended to indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.

[0083] The “heating cavity” mentioned in the text refers to a cavity in which the hollowed-out areas are interconnected, and it may have one or more different diameters, or be composed of one or more different temperature zones.

[0084] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation", "connection" and "linking" should be interpreted broadly. For example, they can be fixed connections, detachable connections, or integral connections; they can be mechanical connections or electrical connections; they can be direct connections or indirect connections through an intermediate medium; and they can be internal connections between two components.

[0085] Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.

[0086] In the description of this invention, unless otherwise stated, "a plurality of" means two or more.

[0087] To achieve a simpler, more intuitive, and realistic simulation of the vapor deposition performance of vacuum-deposited materials on a mass production line using only a small amount of material, this invention discloses a vacuum-deposited material mass production performance evaluation device. This device can simulate the thermal stability performance of a large amount of material under long-term high-temperature vapor deposition conditions in a high vacuum on a mass production line using only a small amount of vacuum-deposited material. It can simply, intuitively, and effectively evaluate the mass production performance of vacuum-deposited materials, avoiding adverse effects or losses on production.

[0088] The following is combined with Fig. 1a-Fig. 1d , Fig. 2a-2e , Fig. 3-Fig. 5 This invention is used to demonstrate the vacuum coating material mass production performance evaluation device. Fig. 1a-Fig. 1d ,Fig. 2a-2e , Fig. 3-Fig. 5 This is merely a non-limiting example, and the figures are not necessarily drawn to scale. The present invention provides a device for evaluating the mass production performance of vacuum-coated materials. Fig. 1a For example, it includes at least one vacuum device 110, at least one heating device 120, and at least one vertically arranged material container 130.

[0089] The vacuum coating material mass production performance evaluation device 100 disclosed in this invention includes at least one vacuum device 110, such as... Fig. 1a-Fig. 1d As shown, it mainly includes vacuum equipment and vacuum piping connecting the material container and the vacuum equipment. Specifically, as... Fig. 1b As shown, the vacuum equipment can be various suitable vacuum pumps, including a mechanical pump 119 and a molecular pump 118. The molecular pump 118 and mechanical pump 119 can also be replaced by other vacuum pumps, such as condenser pumps. The mechanical pump 119 and molecular pump 118 are connected to the material container 130 via a gas guide pipe 114. The mechanical pump 119 is typically positioned after and connected to the molecular pump 118. Furthermore, a cold trap (not shown in the figure) can be configured before the molecular pump 118. Adding a cold trap increases the ultimate vacuum of the entire device and prevents material from being drawn into the pump. During operation, the vacuum level of the material container 130 is controlled by the mechanical pump 119 and the molecular pump 118, and the vacuum level achieved during operation is ≤1.0*10⁻⁶. -3 Pa, preferably, the vacuum level achieved during operation is ≤1.0*10 Pa. -4 Pa. The vacuum pipeline includes a connector section and a gas guide pipe 114. The connector section is used to connect to the material container 130. The connector section can use any suitable connecting component, including but not limited to nuts 111, reducers 112, clamps 113, threads, sealing rings, flanges, etc. In addition, the gas guide pipe 114 can also have a vacuum degree measuring device 115, as well as valves 116 and venting valves 117 for controlling the vacuum degree. The vacuum degree measuring device 115 can be a full-range vacuum gauge or other available vacuum monitoring equipment. The vacuum degree measuring device is used to monitor the vacuum degree inside the material container 130 to ensure a high vacuum state within the system. Furthermore, the vacuum degree measuring device can also have a matching display device to more intuitively display the vacuum degree data within the system.

[0090] The vacuum coating material mass production performance evaluation device 100 disclosed in this invention includes at least one vertically arranged material container 130, wherein the at least one material container 130 is tubular, and for considerations of ease of processing and mechanical strength, the cross-section of the material container 130 is preferably circular, such as... Fig. 2aAs shown, it includes at least part A 1301 and part B 1302. Part B 1302 is used to hold the sample to be tested. After the sample is sublimated from part B 1302, it can be cooled and deposited on part A 1301. Part A 1301 and part B 1302 of the material container 130 have concentric axes and are connected to each other. The end of part B 1302 away from the connection between part A 1301 and part B 1302 is closed (i.e., the bottom). The end of part A 1301 away from the connection between part A 1301 and part B 1302 (i.e., the top) is connected to the vacuum device 110. After the material container 130 is connected to the vacuum device 110, the material container 130 is in a vertical state. That is, when in the working state, the material container 130 is in a vertical state, and part A 1301 is located above part B 1302. The material container 130 preferably has graduations on its tube wall, which makes it easier to read the thickness of the material buildup and the thickness of any ash particles that may be generated. Compared to horizontal or tilted placement, vertical placement of the material container 130 makes it easier to intuitively read information such as the height of the ash particles and the height of the material from the graduations. Furthermore, since ash particles are generally generated or accumulated on the material surface, vertical placement maximizes the ash height, facilitating observation and recording, and also making it easier to extract the ash particles for physicochemical analysis and testing. In addition, the material container 130 is made of a transparent material, preferably a transparent rigid material, and more preferably quartz or glass. Its tube wall needs to have a certain thickness to further ensure the mechanical strength of the material container and prevent damage under high vacuum conditions. A tube wall that is too thin is difficult to process, while a tube wall that is too thick will affect heat transfer performance; therefore, the preferred tube wall thickness is 1~4 mm.

[0091] Specifically, the material container 130 can be schematically described as follows: Fig. 2a~2e As shown. Fig. 2a The material container 1301 shown has part A 1301 and part B 1302. Part A has a diameter D. A The portion of part B that is furthest from the junction of parts A and B is the main body, and the main body has a diameter D. B After the material cools and deposits on the pipe wall in section A, some material particles may fall off due to gravity or vibration. If these particles fall onto the surface of the material to be tested in section B, they will disrupt any existing ash layering, thus affecting subsequent recording and testing. One of the core contents of this invention is how to cleverly avoid this situation: In this invention, a special structural design is creatively added to the material container 130 to catch any material particles that may fall from section A.

[0092] One way is as follows Fig. 2a As shown, the D of the material container 130 A / D B>1, thus forming a platform-shaped area at the connection between the bottom of part A and part B. When material deposited on the wall of pipe A falls, it will land on the platform-shaped area at the bottom of part A, and not inside part B. Preferably, D A / D B ≥1.5.

[0093] Another feasible approach is as follows Fig. 2b As shown, the top of part B 1302 protrudes into the interior of part A 1301 by a certain distance. The height of this protrusion can be 1-20 mm, preferably 5-20 mm, and more preferably 10-20 mm. This design allows part B to form a barrier 1303 at the connection between part A and part B. The barrier 1303 and the pipe wall of the bottom area of ​​part A form a trough-like space, which can catch particles or droplets that fall from the material deposited in part A.

[0094] Similarly, the aforementioned construction site fence 1303 can also be... Fig. 2c As shown, in this case, the portion of part B furthest from the closed end has a diameter D. b And D b Less than D A This creates a structure with a varying diameter at the junction of part A 1301 and part B 1302, effectively preventing potentially falling material particles from damaging the ash layer. It should be noted that 1303 belongs to part B and has a variable diameter. Alternatively, as... Fig. 2d As shown, its D A / D B When the value is 1, to prevent material from falling back, a barrier 1303 is designed at the connection between part A 1301 and part B 1302. Alternatively, as shown below... Fig. 2e As shown, in Fig. 2d Based on this, at the connection between part A 1301 and part B 1302, in addition to designing a barrier 1303, the diameter is further narrowed to further control the evaporation rate of the material under test at high temperatures. Fig. 2a-Fig. 2e This is a schematic diagram of the structure of material container 130, and is not intended to limit it. Different material containers can be selected for different samples to achieve better experimental results.

[0095] In addition, in order to use as little material as possible while ensuring the material stacking effect, the diameter of section B 1302 should not be too large, and the main pipe diameter D of section B 1302 should be... B ≤30 mm, preferably, D B ≤20 mm, more preferably, D B≤10 mm. The diameter of part A 1301 should not be too large. If the diameter of part A 1301 is too large, the material to be tested will be deposited as a very thin layer in part A 1301, which is not conducive to the subsequent removal of the sublimated material. Therefore, the preferred size is D. A / D B ≤3. The length of the main body of part B 1302 should not be too long, generally ≤100 mm, preferably ≤60 mm. To facilitate the sublimation deposition of the material and to make it easier to collect the material, the length of part A 1301 should be greater than or equal to 1-2 times the length of part B 1302. Since vacuum coating materials are expensive, the amount of material used should be minimized while ensuring the effect. When D B When the length of part B 1302 is ≤60 mm, the maximum amount of material that the material container 130 can hold is usually no more than 5 g. Obviously, the device of the present invention only requires a small amount of material to make a direct evaluation.

[0096] The material container 130 of the present invention can be integrally formed from part A 1301 and part B 1302, or it can be detachably connected from part A 1301 and part B 1302. In this case, the connection method of part A 1301 and part B 1302 is well known to those skilled in the art and will not be described in detail here. Part B 130 holds the sample to be tested. In the working state, part B 130 is located in the high-temperature zone of the heating device. Part A 1301 of the material container 130 and the area where part A 1301 and part B 1302 are connected are used for material deposition. In the working state, they are located in the low-temperature zone of the heating device. It should be noted that the connection area of ​​part A 1301 and part B 1302 or the part where the enclosure 1303 is located is not part of the main body of part B 1302. In the working state, it is located in the low-temperature zone of the heating device.

[0097] The vacuum coating material mass production performance evaluation device 100 disclosed in this invention further includes at least one heating device 120, wherein the at least one heating device 120 includes at least one heating furnace 121, at least one temperature zone divider 122, and at least one heating chamber 123, as shown below. Fig. 1cAs shown. The heating furnace 121 is equipped with a temperature zone divider 122, which divides the heating chamber 123 into two temperature zones, a and b. Zone a is located above zone b, and zone a is a low-temperature zone, while zone b is a high-temperature zone. The temperature zone divider 122 has a heat insulation function, thus effectively suppressing heat transfer between the two temperature zones a and b, enabling more precise temperature control. The temperature zone divider 122 is well known to those skilled in the art and will not be described in detail here. This device requires the sample to be tested in section B 1302 to be in the high-temperature zone, continuously evaporating / sublimating at a certain temperature. To prevent the sublimated sample from being drawn into the vacuum pump and causing damage to the pump, as described above, a material container section A 1301 (and section B, which serves as the A / B connection or enclosure) is provided and located in the low-temperature zone to cool and deposit the sample sublimated from the main section B. To achieve better deposition results, the temperature of zone b is at least 60 °C higher than that of zone a, preferably at least 100 °C higher.

[0098] Furthermore, the sublimation temperature of general organic materials (or other vacuum-coated materials) is below 1000 ℃. Therefore, the temperature control range of the heating device 120 is from room temperature to 1000 ℃. To achieve more precise temperature control, the temperature control accuracy is less than or equal to ±3 ℃, preferably less than or equal to ±1 ℃. The material container 130 operates within the heating chamber 123. Therefore, the smaller the gap between the heating chamber wall and the material container 130, the better for heat transfer, so that the temperature of the heating chamber 123 is approximately equal to the temperature of the material container 130 and the material sample inside it. The heating chamber 123 of the heating device 120 includes at least two hollow areas, C1 and C2. C1 corresponds to temperature zone a, used to accommodate part A 1301 of the material container 130; C2 corresponds to temperature zone b, used to accommodate part B 1302 of the material container 130. It should be noted that although the portion corresponding to the aforementioned enclosure belongs to part B 1302, it does not belong to the main pipe diameter portion (main body) of part B 1302. The temperature zone a corresponding to its heating device, C1, is located above C2 and has a diameter D. C1 and D C2 And satisfy the following conditions: D C1 >D A ≥D C1 -10 mm and D C2 >D B ≥D C2 -10 mm; preferably, D C1 >D A ≥D C1 -5 mm and D C2 >D B ≥D C2 -5 mm; more preferably, D C1 >D A ≥D C1-3 mm and D C2 >D B ≥D C2 -3 mm. Fig. 1d Another heating device 120 is shown, in which the diameters of part a and part b of the heating cavity 123 can be substantially the same, which is more suitable for... Fig. 2d and Fig. 2e The structure of the material container 130 is shown.

[0099] Furthermore, in the working state, the relative position of the material container and the heating chamber is fixed. To achieve this, there are multiple feasible ways to install and open the mass production performance evaluation device of the present invention. That is, there are multiple feasible ways to install the material container 130 in place. For example, the heating device 120 is composed of two parts joined together, so that the heating device 120 can be opened. Fig. 3 As shown, the heating device can be opened via a sliding rail, allowing the material container 130 to be connected to the vacuum device 110 first, and then the heating device 120 to be closed, at which point the material container 130 is in the working position. Alternatively, the heating device 120 can be a single unit, without needing to open its interior, but the heating device 120 or the vacuum device 110 connected to the material container can be moved / adjusted. For example, the heating device 120 can have a lifting device, or the vacuum device 110 connected to the material container 130 can be equipped with a lifting device. These lifting devices can be located outside the heating device 120, allowing adjustment of the relative position of the heating device 120 and the material container 130 to the working state. The lifting device can be a spring, screw, cylinder, or other available lifting device for ease of operation. The installation and use of these lifting devices are well known to those skilled in the art and will not be described in detail here. An observation window can be provided on the heating device 120, allowing for observation of the contents of the material container 130 at any time while the mass production performance evaluation device of this invention is in operation.

[0100] like Fig. 4 As shown, the vacuum coating material mass production performance evaluation device of the present invention can also include multiple heating chambers 123 in a heating device 120 (the figure shows the case where a heating device 120 includes three heating chambers 123). For the same test sample that needs to be tested in parallel or multiple test samples with the same heating temperature, they can be tested simultaneously, which greatly improves the efficiency of the work.

[0101] like Fig. 5As shown, the vacuum coating material mass production performance evaluation device of the present invention may also include multiple heating devices 120, and each heating device 120 includes at least one heating chamber 123 (the figure illustrates an evaluation device including two heating devices 120, one heating device 120 including one heating chamber 123, and the other heating device 120 including two heating chambers 123). Since each heating chamber 123 can independently control the temperature, multiple samples of the same test material can be tested in parallel, and multiple test materials with different heating temperatures can be tested simultaneously, which can greatly improve the efficiency of the work.

[0102] like Fig. 6 The diagram shown is a flowchart of a method for evaluating the mass production performance of vacuum-coated materials using the apparatus described above. Details are as follows:

[0103] The first step is to obtain a sample of the vacuum coating material to be tested. After obtaining the material, its physical properties can be measured, including but not limited to purity, melting point, glass transition temperature, and decomposition temperature. These data reflect some basic properties of the material and can serve as a basis for subsequent data comparison.

[0104] Step two: Fill the material (sublimated product) into the material container and record the initial mass M0 of the vacuum coating material sample to be tested. To prevent the material from overflowing the material container and to save material, the maximum amount of filler generally should not exceed 80% of the height of part B of the material container (excluding the enclosure); preferably, not more than 60%; more preferably, not more than 50%. Record the height H0 of the material to be tested inside the material container.

[0105] The material container 130 can then be installed as follows: Place the material container 130 in the heating chamber 123 of the heating device 120, adjust the relative position of the material container 130 and the heating device 120, and align the connection between part A 1301 and part B 1302 of the material container with the temperature zone separation of the heating device. Then, fix the material container 130 to the gas guide pipe 114 to connect to the vacuum device 110. Alternatively, the material container 130 can be connected to the gas guide pipe 114 first, and then moved to a suitable position in the heating chamber 123.

[0106] Before starting the work, it is necessary to determine the heating temperature T and baking time t required for the mass production performance evaluation of this material under test using the evaluation device of the present invention.

[0107] Depending on the actual situation, the heating temperature T of the material to be tested can be determined according to any of the following methods:

[0108] 1. If the material under test has been used in a mass production line vapor deposition machine and has vapor deposition experience on the mass production line (this mass production vapor deposition experience means that the material has been vapor deposition on the mass production vapor deposition machine for a period of time, such as 1-2 days. This process is not a real mass production process, but only a test. The purpose is usually to obtain data on the vapor deposition rate, vapor deposition temperature, etc. of the material or to make experimental panels to test performance), then T is the actual vapor deposition temperature or the average value of the actual vapor deposition temperature on the mass production vapor deposition machine of the material under test.

[0109] 2. If the material to be tested has not been used in a mass production vapor deposition machine, but only in a research and development vapor deposition machine, the vapor deposition temperature on the research and development vapor deposition machine can be used as the reference temperature. A certain temperature ΔT is added to this reference temperature, such as 15℃, 30℃, 45℃, etc., until the temperature at which ash content or abnormalities appear is determined; this temperature is the heating temperature T. Therefore, T is the vapor deposition temperature of the material on the research and development vapor deposition machine + ΔT. If ΔT is greater than 75℃ and there is still no ash content or abnormalities, the material is considered to have good thermal stability. In this method, material abnormalities refer to a significant change in material color, such as turning black.

[0110] The baking time t can be determined using any of the following methods, depending on the requirements:

[0111] 1.t can be 7 days, 10 days, or 14 days;

[0112] 2.t represents the time during which ash or abnormalities appear in the material under test during sublimation on the mass production performance evaluation device of this invention. In this method, material abnormalities refer to a significant change in the material's color, such as turning black.

[0113] Obviously, the steps of determining the heating temperature T and baking time t can be completed before step five, "heating to a certain temperature and continuing to bake for a certain time".

[0114] After ensuring valve 116 is unobstructed and closing vent valve 117, a vacuum needs to be created. Typically, a mechanical pump is used first to create a vacuum, and once the vacuum level is ≤10 Pa, a molecular pump is used to further create a vacuum level ≤1.0*10 Pa. -3 Pa.

[0115] After the vacuum level reaches the working conditions, the heating temperature of the heating device 120 is set so that the temperature of region b in the heating device 120 rises to the heating temperature T, heating the sample to be tested placed in the main body of part B 1302 of the material container 130; and the temperature of temperature zone a in the heating device 120 is set to ≤ T-60 ℃, preferably, the temperature of temperature zone a is ≤ T-100 ℃; in this way, part A 1301 of the material container 130 and the area where part A 1301 and part B 1302 connect are in the low temperature zone, and the main body of part B 1302 is in the high temperature zone, thereby forming a temperature gradient, which allows the material to be tested to sublimate and deposit on the tube wall of part A 1301 of the material container 130.

[0116] The material is baked at a constant temperature for a time t. During this period, the changes in the state of the material in the container can be observed through the observation window, such as changes in material morphology, ash production, color changes, and the amount of remaining material.

[0117] Afterwards, heating is stopped and the heating device 120 is allowed to cool to room temperature. Then, the molecular pump 118 and mechanical pump 119 are turned off in sequence, the vent valve 117 is opened to break the vacuum, and the material container 130 is removed. The appearance (color, shape, whether ash is produced, etc.) of the material in the material container 130 can be observed and recorded, and written and / or photographic records can be made. The accumulation height H1 of the remaining material is read or measured. If ash is present, the accumulation height H2 of the ash is read or measured, and the mass M1 of the remaining material is weighed. Clearly, after completing the above experiment, if the ash accumulation height H2 is large, or the appearance of the remaining material is poor, it can be preliminarily judged that this test material is not suitable for mass production; conversely, if H2 is small, or the appearance of the remaining material is good (color, shape, etc., changes are not visible to the naked eye), it can be preliminarily judged that this test material is relatively suitable for mass production.

[0118] Furthermore, commercially available vacuum coating material samples and the vacuum coating material sample to be tested can be taken and evaluated using the mass production performance evaluation device of this invention. The thermal stability and mass production performance of the vacuum coating material sample to be tested can be evaluated by comparing the quality of the materials. For example, if the vacuum coating material to be tested produces less ash after the experiment than the commercial material of the same weight / volume, then it can be determined that the mass production performance of the material to be tested is superior to that of the commercial material, and it has mass production potential.

[0119] Further physical property tests can be conducted on the remaining material, including but not limited to purity, melting point, glass transition temperature, and decomposition temperature. If the material being tested produces ash, further physical property tests can be conducted on the ash, including but not limited to purity, melting point, glass transition temperature, and decomposition temperature. By comparing the physical property parameters of the remaining material and ash with those of the material being tested before the experiment, the changes in the material's properties under long-term high-temperature vapor deposition can be evaluated. Furthermore, the remaining material can be verified through device testing to more accurately determine whether the material's properties will affect device performance, thereby evaluating its mass production performance. The average sublimation rate of the vacuum-deposited material, v=(M0-M1) / t, can also be calculated as a reference for the mass production vapor deposition rate. Through a series of experiments, the ash height at different average sublimation rates can be obtained. If the vapor deposition rate required for mass production is known, the ash content that the material may produce under mass production conditions can be simulated. Parameters such as the purity, melting point, glass transition temperature, and decomposition temperature of the material before and after the experiment can also serve as important indicators for evaluating the material.

[0120] The vacuum coating material mass production performance evaluation device disclosed in any of the foregoing embodiments of the present invention can also be used as a micro-volume (mass ≤ 1 g; preferably, mass ≤ 0.5 g; more preferably, mass ≤ 0.1 g) material sublimation device. That is, the vacuum coating material mass production performance evaluation device is a micro-volume material sublimation device, and the specific usage method is as follows:

[0121] Weigh a certain amount of material to be sublimated and add it to the material container 130. The maximum amount of filler in the material container 130 shall not exceed 80% of the volume of part B 1302 of the material container. After the material container is installed in place, evacuate to the working vacuum level. Use the heating device 120 to heat part B 1302 until the material begins to sublimate. Control the heating device to create a temperature gradient between part A 1301 and part B 1302, so that the sublimated material is deposited in part A 1301 of the material container. Maintain the high temperature of part B 1302 until sublimation is complete. Stop heating, cool down, remove the material container 130, and collect the sublimated material deposited in part A 1301.

[0122] As described above, the vacuum coating material mass production performance evaluation device disclosed in this invention can save materials by using a smaller amount of material for testing, and can more simply, intuitively, and realistically simulate the evaluation of material thermal stability under continuous high-temperature heating and vacuum conditions in a mass production line. Multiple heating chambers can be set in one heating furnace, or multiple heating furnaces can be used to test multiple materials simultaneously, which greatly saves testing time. In addition, the device is small in size and saves space, and can complete more sample tests in a limited space and time, which greatly improves testing efficiency.

[0123] It should be understood that the various embodiments described herein are merely examples and are not intended to limit the scope of the invention. Therefore, as will be apparent to those skilled in the art, the claimed invention may include variations of the specific embodiments and preferred embodiments described herein. Many of the materials and structures described herein can be substituted with other materials and structures without departing from the spirit of the invention. It should be understood that various theories regarding why the invention works are not intended to be limiting.

Claims

1. A device for evaluating the mass production performance of vacuum-coated materials, comprising: At least one material container, at least one vacuum device and at least one heating device; The material container is tubular and comprises at least part A and part B; part A has a diameter D. A One end of part B is closed, and the other end of part B is connected to part A. The portion of part B furthest from the closed end has a diameter D. b And D b Less than D A The end of part A that is furthest from the connection between part A and part B is connected to the at least one set of vacuum devices, and the material container is in a vertical position. One end of part B, which connects to part A, protrudes a certain distance into part A to form a barrier. The heating device includes at least one heating chamber C and is capable of accommodating a vertically placed material container.

2. The vacuum coating material mass production performance evaluation device as described in claim 1, wherein, The portion of part B that is furthest from the junction of parts A and B is the main body, and the main body has a diameter D. B And D A / D B ≥ 1.

3. The vacuum coating material mass production performance evaluation device as described in claim 2, wherein, D B / D b ≥ 1。 4. The vacuum coating material mass production performance evaluation device as described in claim 1 or 2, wherein, The B portion has a uniform diameter, or the end of the B portion that connects to the A portion has a change in diameter.

5. The vacuum coating material mass production performance evaluation device as described in claim 1, wherein, Part A and Part B are concentric.

6. The vacuum coating material mass production performance evaluation device as described in claim 2, wherein, The D B ≤30 mm.

7. The vacuum coating material mass production performance evaluation device as described in claim 6, wherein, The D B ≤20 mm.

8. The vacuum coating material mass production performance evaluation device as described in claim 6, wherein, The D B ≤10 mm.

9. The vacuum coating material mass production performance evaluation device as described in claim 1, wherein, The length of part B is ≤100mm, and the length of part A is greater than or equal to the length of part B.

10. The vacuum coating material mass production performance evaluation device as described in claim 1, wherein, The material container has graduations on its tube wall.

11. The vacuum coating material mass production performance evaluation device as described in claim 10, wherein, The tube wall of section B is marked with graduations.

12. The vacuum coating material mass production performance evaluation device as described in claim 1, wherein, The material container is made of a transparent material.

13. The vacuum coating material mass production performance evaluation device as described in claim 1, wherein, The material container is made of quartz or glass.

14. The vacuum coating material mass production performance evaluation device as described in claim 1, wherein, The vacuum device includes a vacuum device and a vacuum pipeline connecting the material container to the vacuum device.

15. The vacuum coating material mass production performance evaluation device as described in claim 2, wherein, The heating chamber C is a cylindrical cavity.

16. The vacuum coating material mass production performance evaluation device as described in claim 15, wherein, The heating chamber C comprises at least two parts, C1 and C2, each with independently controllable temperature and a diameter D. C1 and D C2 And D C1 >D A ≥D C1 -10 mm, D C2 >D B ≥D C2 -10 mm.

17. The vacuum coating material mass production performance evaluation device as described in claim 16, wherein, D C1 >D A ≥D C1 -5mm, D C2 >D B ≥D C2 -5 mm.

18. The vacuum coating material mass production performance evaluation device as described in claim 1, wherein, The at least one heating device includes a plurality of heating chambers, each of which independently has the same or different shapes and sizes.

19. The vacuum coating material mass production performance evaluation device as described in claim 1, wherein, The mass production performance evaluation device further includes multiple heating devices, each of which includes at least two temperature zones, and each temperature zone can be independently controlled in temperature.

20. The vacuum coating material mass production performance evaluation device as described in claim 19, wherein, The multiple heating devices are paired with a vacuum device.

21. The vacuum coating material mass production performance evaluation device as described in claim 1, wherein, The heating device further includes a lifting device and / or an observation window.

22. A method for evaluating the mass production performance of vacuum-deposited materials using the vacuum-deposited material mass production performance evaluation apparatus as described in claim 1, comprising the following steps: Step 1: Obtain the material to be tested. Step two: Fill the material to be tested into the material container and record the results. Step 3: Install the material container in place. Step four, vacuum extraction. Step 5: Heat to a certain temperature and continue baking for a certain period of time. Step six: Record data, including measuring and recording the height of the ash content.

23. The method of claim 22, wherein, The method further includes the step of determining a heating temperature T, wherein the heating temperature T is determined according to any of the following methods: (1) The heating temperature T is the vapor deposition temperature of the material to be tested on the mass production vapor deposition machine; (2) The heating temperature T is the vapor deposition temperature of the material to be tested on the vapor deposition machine plus a certain temperature ΔT; Wherein, ΔT ≤ 75 ℃.

24. The method of claim 22, wherein, The method further includes the step of determining a baking time t, wherein the baking time t is determined according to any of the following methods: (1) The baking time t is 7 days, 10 days or 14 days; (2) The baking time t is the time when the material to be tested exhibits ash or abnormalities during sublimation on the mass production performance evaluation device.

25. The method of claim 22, wherein, The method further includes measuring the physical properties of the material under test before and after the experiment and / or recording the device test results of the material under test.

26. The method of claim 22, wherein, The data recording step further includes calculating the average sublimation rate v.

27. The use of the vacuum coating material mass production performance evaluation device as described in any one of claims 1-21 as a micro-sublimation device, wherein, The micro-sublimation equipment is used to sublimate less than 1 gram of vacuum-coated material.

28. The use as described in claim 27, wherein the micro-sublimation apparatus is used to sublimate up to 0.5 grams of vacuum-deposited material.

29. The use as described in claim 27, wherein the micro-sublimation apparatus is used to sublimate less than 0.1 gram of vacuum-deposited material.

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