Device for analyzing residual solvents through re-dissolution
The device efficiently re-dissolves and analyzes residual solvents in thin films or patterns, addressing the challenges of incomplete solvent removal in solution processes, enhancing reliability and safety while enabling material recycling.
Patent Information
- Application Number
- PCT/KR2025/002150
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2024-02-21
- Filing Date
- 2025-02-13
- Publication Date
- 2025-08-28
AI Technical Summary
Existing solution processes for forming thin films or patterns leave residual solvents that are difficult to remove completely, requiring lengthy processes and are harmful to health and the environment, with no efficient method to measure or verify the effectiveness of solvent removal.
A device for analyzing residual solvent through re-dissolution, comprising a collection unit with a nozzle and pressure control system to re-dissolve and collect thin films or patterns, and an analysis unit to inspect the solvent content, enabling rapid and reliable detection of residual solvents.
The device allows for rapid and complete re-dissolution of thin films or patterns, improving the reliability and efficiency of solvent inspection, reducing health and environmental risks, and facilitating the recycling of materials.
Smart Images

Figure KR2025002150_28082025_PF_FP_ABST
Abstract
Description
Residual solvent analysis device through redissolution
[0001] The present invention relates to a residual solvent analysis device, and more particularly, to a device for analyzing residual solvent by re-dissolving a thin film or pattern formed by a solution process.
[0002] In general, a solution process is a process of forming a thin film or pattern using a solution of a specific substance dissolved in a solvent. It is used in various fields because it has the advantage of being able to apply various processes utilizing the properties of liquid substances.
[0003] In these solution processes, most solvents are used to dissolve or disperse specific substances in liquid form for the convenience of work, and do not form thin films or patterns as a result of the solution process.
[0004] Rather, it is better to remove the solvent from the thin film or pattern because it has a negative effect on the properties, shape, or durability of the formed thin film or pattern.
[0005] Furthermore, since the solvent in the solution process is selected for convenience of operation, substances harmful to the human body and the environment are often used, and solvents remaining in the thin film or pattern formed through the solution process can harm the health of the user and pollute the environment.
[0006] For example, in the case of perovskite materials, which are widely used in the manufacture of electronic devices due to their characteristics that allow solution processes to be applied, it is very important to properly remove residual solvents.
[0007] At this time, the solvent can be removed through natural evaporation after the solution process, but this method has the drawback of requiring a significant amount of time for the solvent to be removed. Therefore, a separate residual solvent removal process is typically performed, but it is very difficult to completely remove the solvent within the thin film or pattern, given the influence of the thin film or pattern shape.
[0008] Accordingly, if the subsequent process for removing residual solvent becomes too long or the process cost increases, the efficiency of the overall solution process decreases, so optimization of the residual solvent removal process is necessary.
[0009] However, since it is very difficult to measure the amount of solvent removed during the residual solvent removal process or to measure the solvent remaining after the residual solvent removal process, it is very difficult to optimize the residual solvent removal process and verify the effectiveness of the residual solvent removal process.
[0010] The present invention is intended to solve the problems of the prior art described above, and its purpose is to provide a device for analyzing the solvent remaining by re-dissolving a thin film or pattern formed by a solution process.
[0011] In order to achieve the above object, the present invention provides a device for analyzing residual solvent through re-dissolution, which is a device for examining a solvent remaining in a thin film or pattern formed through a solution process and proceeding to a residual solvent removal process, the device comprising: a collection unit for re-dissolving and collecting the thin film or pattern; and an analysis unit for analyzing the collected test sample to examine the residual solvent, wherein the collection unit comprises: a nozzle unit including a discharge nozzle for discharging a standard reagent capable of dissolving the thin film or pattern and performing a residual solvent test, and a suction nozzle for collecting a solution in which the thin film or pattern is dissolved by the standard reagent; a first pressure control unit for applying positive pressure to the discharge nozzle and negative pressure to the suction nozzle; a solution storage unit including a first reservoir for storing a solution discharged through the discharge nozzle and a second reservoir for storing a solution collected through the suction nozzle; And it includes a solution circulation unit that transfers and circulates the solution stored in the second reservoir to the first reservoir, and the analysis unit includes a sample storage unit that stores a test sample to be subject to residual solvent test; and an analyzer that receives the test sample stored in the sample storage unit and performs a residual solvent test.
[0012] The above discharge nozzle may be a needle-type discharge nozzle.
[0013] The above discharge nozzle may be a multi-needle type discharge nozzle.
[0014] It is preferable that the above first pressure control unit can generate positive pressure up to 500 kPa.
[0015] It is preferable that the above first pressure control unit be capable of generating negative pressure up to 50 kPa.
[0016] The solution stored in the first reservoir can be transferred to the sample storage unit by the positive pressure applied to the first reservoir.
[0017] The above analysis unit may include a second pressure control unit that applies pressure to the sample storage unit.
[0018] It is preferable that the above second pressure control unit be capable of generating positive pressure up to 100 kPa.
[0019] It is preferable that the above second pressure control unit be capable of generating negative pressure up to 10 kPa.
[0020] The above sample storage unit is connected to a syringe-type sample injection unit, and the analyzer may be equipped with a syringe-type sample injection port.
[0021] It may further include a moving device for moving the location of the sample storage unit.
[0022] It may further include a saturated vapor pressure maintenance cover covering the upper portion of the location where re-dissolution and suction are performed by the discharge nozzle and the suction nozzle.
[0023] The present invention, configured as described above, has the effect of enabling inspection by rapidly re-dissolving and sucking a thin film or pattern formed through a solution process and progressing to a residual solvent removal process through a discharge nozzle and a suction nozzle connected to a pressure control unit, thereby performing inspection by re-dissolving a significant amount or the entire thin film or pattern formed on a substrate.
[0024] In addition, by re-dissolving a large portion of the thin film or pattern formed on the substrate and performing an inspection for residual solvent, the difficulty of the inspection is reduced while the reliability of the inspection results is improved, which has the excellent effect of improving the reliability of the inspection results.
[0025] Figure 1 is a schematic diagram illustrating the configuration of a residual solvent analysis device through redissolution according to an embodiment of the present invention.
[0026] Figure 2 is a schematic diagram illustrating a sampling section of a residual solvent analysis device through redissolution according to the first embodiment of the present invention.
[0027] FIG. 3 is a drawing for explaining the structure and operation of a nozzle section in a residual solvent analysis device through re-dissolution according to the first embodiment of the present invention.
[0028] Figure 4 is a schematic diagram illustrating an analysis unit of a residual solvent analysis device through redissolution according to an embodiment of the present invention.
[0029] FIG. 5 is a drawing showing a nozzle section of a residual solvent analysis device through redissolution according to a second embodiment of the present invention.
[0030] FIG. 6 is a drawing showing a nozzle section of a residual solvent analysis device through redissolution according to a third embodiment of the present invention.
[0031] FIG. 7 is a drawing showing a configuration in which a saturated vapor pressure maintenance cover is added to the nozzle section of a residual solvent analysis device through redissolution according to the fourth embodiment of the present invention.
[0032] FIG. 8 is a drawing showing a configuration in which a saturated vapor pressure maintenance cover is added to the nozzle section of a residual solvent analysis device through re-dissolution according to the fifth embodiment of the present invention.
[0033] FIG. 9 is a drawing showing a configuration in which a saturated vapor pressure maintenance cover is added to the nozzle section of a residual solvent analysis device through redissolution according to the sixth embodiment of the present invention.
[0034] An embodiment of the present invention will be described in detail with reference to the attached drawings.
[0035] However, the embodiments of the present invention may be modified in various other forms, and the scope of the present invention is not limited to the embodiments described below. The shapes and sizes of elements in the drawings may be exaggerated for clearer explanation, and elements indicated by the same symbols in the drawings are the same elements.
[0036] Throughout the specification, when a part is said to be "connected" to another part, this includes not only the cases where it is "directly connected" but also the cases where it is "electrically connected" with another element in between. Furthermore, when a part is said to "include" or "comprise" a component, this does not mean that it excludes other components, but rather that it can include or comprise other components, unless otherwise specifically stated.
[0037] Additionally, terms such as "first," "second," etc. are intended to distinguish one component from another and should not be construed as limiting the scope of the rights. For example, the first component may be referred to as the second component, and similarly, the second component may also be referred to as the first component.
[0038]
[0039] Figure 1 is a schematic diagram illustrating the configuration of a residual solvent analysis device through redissolution according to an embodiment of the present invention.
[0040] A residual solvent analysis device through re-dissolution according to an embodiment of the present invention is composed of a collection unit (100) and an analysis unit (200).
[0041]
[0042] The collection unit (100) is a component that collects an analysis sample by re-dissolving a thin film or pattern formed through a solution process and completing a residual solvent removal process.
[0043] FIG. 2 is a schematic diagram for explaining a sampling unit of a residual solvent analysis device through re-dissolution according to a first embodiment of the present invention, and FIG. 3 is a diagram for explaining the structure and operation of a nozzle unit in a residual solvent analysis device through re-dissolution according to a first embodiment of the present invention.
[0044] The collection unit (100) includes a nozzle unit (110), a first pressure control unit (120), a solution storage unit (130), and a solution circulation unit (140).
[0045] The nozzle section (110) includes a discharge nozzle (112) for discharging a standard reagent for dissolving a thin film or pattern to be collected, and a suction nozzle (114) for suctioning and recovering a solution re-dissolved by the discharged standard reagent.
[0046] At this time, the standard reagent is the standard reagent used for residual solvent analysis of the collected analysis sample, but a solvent-compatible reagent that is compatible with the base that constitutes the thin film or pattern is used so that the thin film or pattern that has undergone the residual solvent removal process can be re-dissolved. At this time, not only the standard reagent can be used, but other types of reagents can also be used, and the base solvent used in the process of forming the thin film to be re-dissolved can be applied.
[0047] The first pressure control unit (120) is used to apply positive pressure during the process of discharging the standard reagent from the discharge nozzle (112) of the nozzle unit (110) and to apply negative pressure during the process of sucking the redissolved solution from the suction nozzle (114) of the nozzle unit (110).
[0048] In this embodiment, since a thin film or pattern formed by a solution process and subjected to a residual solvent removal process is re-dissolved, simply dropping a standard reagent for re-dissolution onto the surface of the thin film or pattern may take too much time for the re-dissolution process. Therefore, the standard reagent discharged from the discharge nozzle (112) of the nozzle unit (110) is configured to be strongly discharged by receiving positive pressure. With this configuration, the standard reagent discharged from the discharge nozzle (112) of the nozzle unit (110) is easily re-dissolved due to the effect of striking the surface of the thin film or pattern.
[0049] At this time, since there is a problem that the time required for the overall residual solvent analysis becomes longer when the time required for re-dissolution and the time required for suction become longer, it is preferable that the first pressure control unit (120) be configured to be able to generate positive pressure up to 500 kPa and negative pressure up to 50 kPa.
[0050] In this way, in this embodiment, both positive pressure for the discharge nozzle (112) and negative pressure for the suction nozzle (114) are required, and the first pressure control unit (120) may be provided with a positive pressure generator and a negative pressure generator separately and connected to each other, or may use one pressure controller capable of generating both positive and negative pressure and connect them separately as a positive pressure transmission line and a negative pressure transmission line.
[0051] Currently, to verify the effectiveness of the residual solvent removal process, the amount of solvent remaining in a thin film or pattern is detected. Due to the difficulty of the re-dissolution process, only a small portion of the entire thin film or pattern is used for testing. However, when the amount of re-dissolution is small, the test difficulty increases, and because the test is performed on a very small portion compared to the entire thin film or pattern, the reliability of the test is lowered.
[0052] In contrast, the present embodiment can quickly re-dissolve and suction a thin film or pattern formed through a solution process and proceeded to a residual solvent removal process through a discharge nozzle (112) and a suction nozzle (114) connected to the first pressure control unit (120) to collect the thin film or pattern, so that a significant amount or the entire thin film or pattern formed on the substrate can be re-dissolved and inspected. Consequently, since more thin films or patterns can be re-dissolved and inspected for residual solvent with a similar amount of time and effort, the difficulty of the inspection can be lowered and the reliability of the inspection results can be improved.
[0053] The solution storage unit (130) includes a first reservoir (132) that stores a standard reagent to be discharged through a discharge nozzle (112) to re-dissolve a thin film or pattern formed through a solution process and proceeded to a residual solvent removal process, and a second reservoir (134) that sucks and stores a solution in which the thin film or pattern is re-dissolved by the discharged standard reagent.
[0054] The first reservoir (132) connected to the discharge nozzle (112) is connected to a positive pressure generator or a positive pressure transmission line, and the second reservoir (134) connected to the suction nozzle (114) is connected to a negative pressure generator or a negative pressure transmission line.
[0055] The solution circulation unit (140) is equipped with a circulation line (142) and a circulation pump (144) to circulate the solution between the first reservoir (132) and the second reservoir (134).
[0056] Specifically, the solution circulation unit (140) transfers the re-dissolved solution stored in the second reservoir (134) to the first reservoir (132) and circulates it, and re-dissolves the re-dissolved solution transferred to the first reservoir (132) through the discharge nozzle (112) to re-dissolve a thin film or pattern, thereby increasing the concentration of the re-dissolved substance in the solution and achieving a concentration effect.
[0057] In general, to detect residual solvent in a solution redissolved with a standard reagent, the concentration of the redissolved substance contained in the solution must be above a certain level (approximately 10% or more). According to the present embodiment, since a thin film or pattern is redissolved by repeatedly using a predetermined amount of the standard reagent, the concentration of the redissolved substance in the solution continuously increases, ultimately eliminating the need for a separate concentration process to generate a test sample.
[0058] Meanwhile, if there is no limit to the concentration of the re-dissolved material, re-dissolution using a large amount of reagent is possible. For example, if a pre-formed perovskite active layer is re-dissolved in liquid form and recovered, concentration adjustment may not be necessary. In this case, the perovskite material in discarded electronic devices can be recycled to recover extremely small amounts of heavy metals harmful to humans and the environment, thereby preventing health and environmental problems.
[0059]
[0060] The analysis unit (200) is a component that performs a test for residual solvent using a test sample that has been re-dissolved and collected.
[0061] Figure 4 is a schematic diagram illustrating an analysis unit of a residual solvent analysis device through redissolution according to an embodiment of the present invention.
[0062] The analysis unit (200) includes a sample storage unit (210), a second pressure control unit (220), and an analyzer (230).
[0063] The sample storage unit (210) stores test samples for performing tests on residual solvents. Since the concentration of the re-dissolved substance included in the test sample must be above a certain level in order to detect residual solvents, the concentration may be adjusted for the solution collected from the collection unit (100). However, as previously described, in the present embodiment, by applying the solution circulation unit (140) in the collection unit (100), a predetermined amount of standard reagent is repeatedly used for re-dissolution, so the concentration of the substance re-dissolved in the standard reagent continuously increases, and in most cases, the solution collected from the collection unit can be used as a test sample without a separate concentration process. If there is no limitation on the concentration of the re-dissolved substance, the sample storage unit (210) may be configured to store the re-dissolved substance using a large amount of reagent.
[0064] Therefore, the process of storing the solution collected from the collection unit (100) in the sample storage unit (210) can be carried out in various ways.
[0065] For example, it is possible to send the solution stored in the first reservoir (132) or the second reservoir (134) of the collection unit (100) to the sample storage unit (210) and store it, and the method of sending the solution stored in the first reservoir (132) or the second reservoir (134) to the sample storage unit (210) is not particularly limited. For example, the first reservoir (132) or the second reservoir (134) and the sample storage unit (210) can be connected by a pipe, and the solution stored in the first reservoir (132) or the second reservoir (134) can be transferred to the sample storage unit (210) using a transfer pump. Alternatively, in a case where the solution is prevented from moving from the first reservoir (132) to the discharge nozzle (112), the solution stored in the first reservoir (132) can be transferred to the sample storage unit (210) by using the positive pressure applied to the first reservoir (132).
[0066] As another example, the first reservoir (132) or the second reservoir (134) of the sampling unit (100) may be used as a sample storage unit (210) in itself. After the process of re-dissolving and collecting a thin film or pattern in the sampling unit (100) is completed, the first reservoir (132) or the second reservoir (134) in which the solution is finally stored may be applied as a sample storage unit (210) of the analysis unit (200) in a subsequent step.
[0067] The second pressure control unit (220) is connected to apply positive or negative pressure to the sample storage unit (210), and can transfer the stored test sample to the analyzer (230) using the positive pressure transmitted to the second pressure control unit (220). The second pressure control unit (220) applies positive pressure to the sample storage unit (210) so that the sample can be injected into the analyzer (230) through the sample injector (212) connected to the sample storage unit (210). It is preferable that the second pressure control unit (220) be configured to be able to generate positive pressure up to 100 kPa and negative pressure up to 10 kPa. Meanwhile, when the first reservoir (132) or the second reservoir (134) is used as a sample storage unit (210), the first pressure control unit (120) can function as the second pressure control unit (220).
[0068] The configuration of the sample injector (212) is not particularly limited, and it is preferable to apply a needle-type sample injector (212) as shown.
[0069] The analyzer (230) is an analysis device that receives a test sample and analyzes the amount of residual solvent. A GC-MS analyzer may be used, but is not limited thereto.
[0070] In order to receive a test sample, a sample injection port (232) corresponding to a sample injector (212) is provided, and in this embodiment, a needle-type sample injection port (232) corresponding to a needle-type sample injector (212) is provided.
[0071] Meanwhile, the residual solvent analysis device through redissolution according to an embodiment of the present invention is preferably used in a state where the thin film or patterned article to be analyzed is placed on the solution process equipment or the residual solvent removal process equipment, rather than performing the inspection by moving the thin film or patterned article to the analysis device of the present invention. Even when the thin film or patterned article is moved to the analysis device of the present invention, the distance is preferably short, and accordingly, the analyzer (230) of the analysis device (200) is often placed at a distance from the sample collection position due to the space provided for the operation of the collection unit (100) and the size of the analysis device. At this time, since the process of injecting the test sample may be difficult if the distance between the sample storage unit (210) and the sample injector (212) becomes long, it is preferable to separately provide a moving device that can move the position of the sample storage unit (210). By separately providing a moving device that can move the location of the sample storage unit (210), as shown in the drawing, the sample storage unit (210) can be moved to the vicinity of the analyzer (230) and the test sample stored in the sample storage unit (210) can be injected into the analyzer (230) through the sample injector (212).
[0072]
[0073] A residual solvent analysis device through re-dissolution according to a second embodiment of the present invention is composed of a collection unit (100) and an analysis unit (200), and the collection unit (100) includes a nozzle unit (110), a first pressure control unit (120), a solution storage unit (130), and a solution circulation unit (140), and the analysis unit (200) includes a sample storage unit (210), a second pressure control unit (220), and an analyzer (230), which are the same as those of the first embodiment.
[0074] The collection unit (100) is a component that collects an analysis sample by re-dissolving a thin film or pattern formed through a solution process and completing a residual solvent removal process.
[0075] The nozzle section (110) includes a discharge nozzle for discharging a standard reagent for dissolving a thin film or pattern to be collected, and a suction nozzle (114) for suctioning and recovering a solution redissolved by the discharged standard reagent.
[0076] However, there are some differences from the first embodiment in the structure of the nozzle applied to the nozzle section (110) of the extraction section (100).
[0077] FIG. 5 is a drawing showing a nozzle section of a residual solvent analysis device through redissolution according to a second embodiment of the present invention.
[0078] The nozzle section (110) of the residual solvent analysis device through re-dissolution according to the second embodiment is characterized by the application of a needle-type discharge nozzle (116), as shown in the drawing.
[0079] As previously discussed, the residual solvent analysis device through re-dissolution of the present embodiment re-dissolves a thin film or pattern that has been formed through a solution process and has gone through a residual solvent removal process, so re-dissolution is not easy simply by dropping a standard reagent on the surface of the thin film or pattern.
[0080] Of course, a first pressure control unit (120) capable of generating a positive pressure of up to 500 kPa for the discharge nozzle that discharges the standard reagent is applied, but the effect of striking the surface of the thin film or pattern may not be sufficient by discharging the standard reagent through the nozzle in a general form.
[0081] To solve this problem, the present embodiment uses a needle-shaped discharge nozzle (116). Since the needle-shaped discharge nozzle (116) has a thinner discharge port than a typical nozzle, the spray pressure of the discharged standard reagent is relatively high. As the spray pressure of the standard reagent increases, the effect of striking the surface of the thin film or pattern increases, resulting in an excellent effect of more smoothly performing re-dissolving.
[0082] The first pressure control unit (120) is used to apply positive pressure during the process of discharging the standard reagent from the needle-shaped discharge nozzle (116) of the nozzle unit (110) and to apply negative pressure during the process of sucking the redissolved solution from the suction nozzle (114) of the nozzle unit (110).
[0083] In this embodiment, a thin film or pattern formed through a solution process and then subjected to a residual solvent removal process can be quickly re-dissolved and collected by suction through a needle-type discharge nozzle (116) and a suction nozzle (114) connected to a first pressure control unit (120), so that a significant amount or the entire thin film or pattern formed on a substrate can be re-dissolved and inspected. Consequently, since more thin films or patterns can be re-dissolved and inspected for residual solvent with a similar amount of time and effort, the difficulty of the inspection can be reduced and the reliability of the inspection results can be improved.
[0084] The solution storage unit (130) includes a first reservoir (132) for storing a standard reagent to be discharged by a needle-shaped discharge nozzle (116) to re-dissolve a thin film or pattern formed by a solution process and proceeding to a residual solvent removal process, and a second reservoir (134) for sucking and storing a solution in which the thin film or pattern is re-dissolved by the discharged standard reagent.
[0085] The solution circulation unit (140) is equipped with a circulation line (142) and a circulation pump (144) to circulate the solution between the first reservoir (132) and the second reservoir (134).
[0086] The sample storage unit (210) stores test samples, etc. for performing tests on residual solvents. Since the concentration of the re-dissolved substance included in the test sample must be above a certain level in order to detect residual solvents, the concentration may be adjusted for the solution collected from the collection unit (100). However, as previously discussed, in the present embodiment, by applying the solution circulation unit (140) to the collection unit (100), a predetermined amount of standard reagent is repeatedly used for re-dissolution, so the concentration of the substance re-dissolved in the standard reagent continuously increases, and in most cases, the solution collected from the collection unit can be used as a test sample without a separate concentration process.
[0087] The second pressure control unit (220) is connected to apply positive or negative pressure to the sample storage unit (210), and the stored test sample can be transferred to the analyzer (230) using the positive pressure transmitted to the second pressure control unit (220).
[0088] The analyzer (230) is an analysis device that receives a test sample and analyzes the amount of residual solvent. A GC-MS analyzer may be used, but is not limited thereto.
[0089]
[0090] A residual solvent analysis device through re-dissolution according to a third embodiment of the present invention is composed of a collection unit (100) and an analysis unit (200), and the collection unit (100) includes a nozzle unit (110), a first pressure control unit (120), a solution storage unit (130), and a solution circulation unit (140), and the analysis unit (200) includes a sample storage unit (210), a second pressure control unit (220), and an analyzer (230), which are the same as the first and second embodiments.
[0091] The collection unit (100) is a component that collects an analysis sample by re-dissolving a thin film or pattern formed through a solution process and completing a residual solvent removal process.
[0092] The nozzle section (110) includes a discharge nozzle for discharging a standard reagent for dissolving a thin film or pattern to be collected, and a suction nozzle (114) for suctioning and recovering a solution redissolved by the discharged standard reagent.
[0093] However, there are some differences in the structure of the nozzle applied to the nozzle section (110) of the extraction section (100) from the first and second embodiments.
[0094] FIG. 6 is a drawing showing a nozzle section of a residual solvent analysis device through redissolution according to a third embodiment of the present invention.
[0095] The nozzle section (110) of the residual solvent analysis device through re-dissolution according to the third embodiment is characterized by the application of a multi-needle type discharge nozzle (118), as shown in the drawing.
[0096] As previously discussed, the residual solvent analysis device through re-dissolution of the present embodiment re-dissolves a thin film or pattern that has been formed through a solution process and has gone through a residual solvent removal process, so re-dissolution is not easy simply by dropping a standard reagent on the surface of the thin film or pattern.
[0097] In the second embodiment, the injection pressure of the standard reagent being discharged is increased using a needle-type discharge nozzle (116), thereby increasing the effect of striking the surface of the thin film or pattern, and enabling re-dissolution to be performed more smoothly. However, the needle-type discharge nozzle (116) has a disadvantage in that the discharge range is narrow.
[0098] To solve this problem, the present embodiment uses a multi-needle type discharge nozzle (118). Since the multi-needle type discharge nozzle (118) has multiple needle-type discharge ports with thinner discharge ports than a general nozzle, it has the advantage of being able to relatively increase the spray pressure of the discharged standard reagent and at the same time widen the range over which the standard reagent is sprayed. By increasing the spray pressure of the standard reagent, the effect of striking the surface of the thin film or pattern is enhanced, so that not only can re-dissolution be performed more smoothly, but also re-dissolution is performed over a wider range, so that the speed of the entire re-dissolution process is excellently increased.
[0099] The first pressure control unit (120) is used to apply positive pressure during the process of discharging the standard reagent from the multi-needle type discharge nozzle (118) of the nozzle unit (110) and to apply negative pressure during the process of sucking the redissolved solution from the suction nozzle (114) of the nozzle unit (110).
[0100] In this embodiment, a thin film or pattern formed through a solution process and then subjected to a residual solvent removal process can be quickly re-dissolved and collected by suction through a multi-needle discharge nozzle (118) and a suction nozzle (114) connected to a first pressure control unit (120), so that a significant amount or the entire thin film or pattern formed on a substrate can be re-dissolved and inspected. Consequently, since more thin films or patterns can be re-dissolved and inspected for residual solvent with a similar amount of time and effort, the difficulty of the inspection can be lowered and the reliability of the inspection results can be improved.
[0101] The solution storage unit (130) includes a first reservoir (132) for storing a standard reagent to be discharged by a multi-needle type discharge nozzle (118) to re-dissolve a thin film or pattern formed by a solution process and proceeding to a residual solvent removal process, and a second reservoir (134) for sucking and storing a solution in which the thin film or pattern is re-dissolved by the discharged standard reagent.
[0102] The solution circulation unit (140) is equipped with a circulation line (142) and a circulation pump (144) to circulate the solution between the first reservoir (132) and the second reservoir (134).
[0103] The sample storage unit (210) stores test samples, etc. for performing tests on residual solvents. Since the concentration of the re-dissolved substance included in the test sample must be above a certain level in order to detect residual solvents, the concentration may be adjusted for the solution collected from the collection unit (100). However, as previously discussed, in the present embodiment, by applying the solution circulation unit (140) to the collection unit (100), a predetermined amount of standard reagent is repeatedly used for re-dissolution, so the concentration of the substance re-dissolved in the standard reagent continuously increases, and in most cases, the solution collected from the collection unit can be used as a test sample without a separate concentration process.
[0104] The second pressure control unit (220) is connected to apply positive or negative pressure to the sample storage unit (210), and the stored test sample can be transferred to the analyzer (230) using the positive pressure transmitted to the second pressure control unit (220).
[0105] The analyzer (230) is an analysis device that receives a test sample and analyzes the amount of residual solvent. A GC-MS analyzer may be used, but is not limited thereto.
[0106]
[0107] A residual solvent analysis device through re-dissolution according to a fourth embodiment of the present invention is composed of a collection unit (100) and an analysis unit (200), and the collection unit (100) includes a nozzle unit (110), a first pressure control unit (120), a solution storage unit (130), and a solution circulation unit (140), and the analysis unit (200) includes a sample storage unit (210), a second pressure control unit (220), and an analyzer (230), which are the same as those of the first embodiment.
[0108] The collection unit (100) is a component that collects an analysis sample by re-dissolving a thin film or pattern formed through a solution process and completing a residual solvent removal process.
[0109] The nozzle section (110) includes a discharge nozzle (112) for discharging a standard reagent for dissolving a thin film or pattern to be collected, and a suction nozzle (114) for suctioning and recovering a solution re-dissolved by the discharged standard reagent.
[0110] In addition, the residual solvent analysis device through re-dissolution according to the fourth embodiment is the same as the first embodiment up to the structure of the nozzle applied to the nozzle section (110) of the sampling section (100), but is different in that it further includes a saturated vapor pressure maintenance cover (300).
[0111] FIG. 7 is a drawing showing a configuration in which a saturated vapor pressure maintenance cover is added to the nozzle section of a residual solvent analysis device through redissolution according to the fourth embodiment of the present invention.
[0112] The nozzle section (110) of the residual solvent analysis device through re-dissolution according to the fourth embodiment further includes a saturated vapor pressure maintenance cover (300) that covers the upper portion of the position where re-dissolution and suction are performed by the discharge nozzle (112) and the suction nozzle (114), as shown.
[0113] The saturated vapor pressure maintenance cover (300) has a through hole (310) in the upper part through which a discharge nozzle (112) and a suction nozzle (114) are inserted, and is configured to cover the upper part and the side surface within a predetermined range where re-dissolution and suction are performed.
[0114] There is a problem that the re-dissolution efficiency decreases when the standard reagent discharged onto the thin film or pattern for re-dissolution evaporates, and the standard reagent may evaporate excessively due to mist, etc., which is generated because the standard reagent is discharged at a relatively high pressure. In particular, since the present embodiment requires minimizing the amount of standard reagent used in the process of obtaining the effect of concentrating the target substance by repeatedly using the standard reagent by applying the solution circulation unit (140), evaporation of the standard reagent may be a problem.
[0115] To solve this problem, in this embodiment, a saturated vapor pressure maintenance cover (300) is added, and evaporation of the standard reagent can be minimized by this saturated vapor pressure maintenance cover (300).
[0116] The first pressure control unit (120) is used to apply positive pressure during the process of discharging the standard reagent from the discharge nozzle (112) of the nozzle unit (110) and to apply negative pressure during the process of sucking the redissolved solution from the suction nozzle (114) of the nozzle unit (110).
[0117] In this embodiment, a thin film or pattern formed through a solution process and then subjected to a residual solvent removal process can be quickly re-dissolved and collected by suction through a discharge nozzle (112) and a suction nozzle (114) connected to a first pressure control unit (120), so that a significant amount or the entire thin film or pattern formed on a substrate can be re-dissolved and inspected. Consequently, since more thin films or patterns can be re-dissolved and inspected for residual solvent with a similar amount of time and effort, the difficulty of the inspection can be reduced and the reliability of the inspection results can be improved.
[0118] The solution storage unit (130) includes a first reservoir (132) that stores a standard reagent to be discharged through a discharge nozzle (112) to re-dissolve a thin film or pattern formed through a solution process and proceeded to a residual solvent removal process, and a second reservoir (134) that sucks and stores a solution in which the thin film or pattern is re-dissolved by the discharged standard reagent.
[0119] The solution circulation unit (140) is equipped with a circulation line (142) and a circulation pump (144) to circulate the solution between the first reservoir (132) and the second reservoir (134).
[0120] The sample storage unit (210) stores test samples, etc. for performing tests on residual solvents. Since the concentration of the re-dissolved substance included in the test sample must be above a certain level in order to detect residual solvents, the concentration may be adjusted for the solution collected from the collection unit (100). However, as previously discussed, in the present embodiment, by applying the solution circulation unit (140) to the collection unit (100), a predetermined amount of standard reagent is repeatedly used for re-dissolution, so the concentration of the substance re-dissolved in the standard reagent continuously increases, and in most cases, the solution collected from the collection unit can be used as a test sample without a separate concentration process.
[0121] The second pressure control unit (220) is connected to apply positive or negative pressure to the sample storage unit (210), and the stored test sample can be transferred to the analyzer (230) using the positive pressure transmitted to the second pressure control unit (220).
[0122] The analyzer (230) is an analysis device that receives a test sample and analyzes the amount of residual solvent. A GC-MS analyzer may be used, but is not limited thereto.
[0123]
[0124] The residual solvent analysis device through re-dissolution according to the fifth embodiment of the present invention is composed of a collection unit (100) and an analysis unit (200), and the collection unit (100) includes a nozzle unit (110), a first pressure control unit (120), a solution storage unit (130), and a solution circulation unit (140), and the analysis unit (200) includes a sample storage unit (210), a second pressure control unit (220), and an analyzer (230), which are the same as the first and second embodiments.
[0125] The collection unit (100) is a component that collects an analysis sample by re-dissolving a thin film or pattern formed through a solution process and completing a residual solvent removal process.
[0126] The nozzle section (110) includes a discharge nozzle for discharging a standard reagent for dissolving a thin film or pattern to be collected, and a suction nozzle (114) for suctioning and recovering a solution redissolved by the discharged standard reagent.
[0127] In addition, the residual solvent analysis device through re-dissolution according to the fifth embodiment is the same as the second embodiment up to the structure in which a needle-type discharge nozzle (116) is applied to the nozzle section (110) of the collection section (100), but is different in that it further includes a saturated vapor pressure maintenance cover (300).
[0128] FIG. 8 is a drawing showing a configuration in which a saturated vapor pressure maintenance cover is added to the nozzle section of a residual solvent analysis device through re-dissolution according to the fifth embodiment of the present invention.
[0129] The nozzle section (110) of the residual solvent analysis device through re-dissolution according to the fifth embodiment further includes a saturated vapor pressure maintenance cover (300) that covers the upper portion of the position where re-dissolution and suction are performed by the needle-shaped discharge nozzle (116) and the suction nozzle (114), as shown.
[0130] The saturated vapor pressure maintenance cover (300) has a through hole (310) in the upper part into which a needle-type discharge nozzle (116) and a suction nozzle (114) are inserted, and is configured to cover the upper part and the side surface within a predetermined range where re-dissolution and suction are performed.
[0131] There is a problem that the re-dissolution efficiency decreases when the standard reagent discharged onto the thin film or pattern for re-dissolution evaporates, and the standard reagent may evaporate excessively due to mist, etc., which is generated because the standard reagent is discharged at a relatively high pressure. In particular, since the present embodiment requires minimizing the amount of standard reagent used in the process of obtaining the effect of concentrating the target substance by repeatedly using the standard reagent by applying the solution circulation unit (140), evaporation of the standard reagent may be a problem.
[0132] To solve this problem, in this embodiment, a saturated vapor pressure maintenance cover (300) is added, and evaporation of the standard reagent can be minimized by this saturated vapor pressure maintenance cover (300).
[0133] The first pressure control unit (120) is used to apply positive pressure during the process of discharging the standard reagent from the needle-shaped discharge nozzle (116) of the nozzle unit (110) and to apply negative pressure during the process of sucking the redissolved solution from the suction nozzle (114) of the nozzle unit (110).
[0134] In this embodiment, a thin film or pattern formed through a solution process and then subjected to a residual solvent removal process can be quickly re-dissolved and collected by suction through a needle-type discharge nozzle (116) and a suction nozzle (114) connected to a first pressure control unit (120), so that a significant amount or the entire thin film or pattern formed on a substrate can be re-dissolved and inspected. Consequently, since more thin films or patterns can be re-dissolved and inspected for residual solvent with a similar amount of time and effort, the difficulty of the inspection can be reduced and the reliability of the inspection results can be improved.
[0135] The solution storage unit (130) includes a first reservoir (132) for storing a standard reagent to be discharged by a needle-shaped discharge nozzle (116) to re-dissolve a thin film or pattern formed by a solution process and proceeding to a residual solvent removal process, and a second reservoir (134) for sucking and storing a solution in which the thin film or pattern is re-dissolved by the discharged standard reagent.
[0136] The solution circulation unit (140) is equipped with a circulation line (142) and a circulation pump (144) to circulate the solution between the first reservoir (132) and the second reservoir (134).
[0137] The sample storage unit (210) stores test samples, etc. for performing tests on residual solvents. Since the concentration of the re-dissolved substance included in the test sample must be above a certain level in order to detect residual solvents, the concentration may be adjusted for the solution collected from the collection unit (100). However, as previously discussed, in the present embodiment, by applying the solution circulation unit (140) to the collection unit (100), a predetermined amount of standard reagent is repeatedly used for re-dissolution, so the concentration of the substance re-dissolved in the standard reagent continuously increases, and in most cases, the solution collected from the collection unit can be used as a test sample without a separate concentration process.
[0138] The second pressure control unit (220) is connected to apply positive or negative pressure to the sample storage unit (210), and the stored test sample can be transferred to the analyzer (230) using the positive pressure transmitted to the second pressure control unit (220).
[0139] The analyzer (230) is an analysis device that receives a test sample and analyzes the amount of residual solvent. A GC-MS analyzer may be used, but is not limited thereto.
[0140]
[0141] The residual solvent analysis device through redissolution according to the sixth embodiment of the present invention is composed of a collection unit (100) and an analysis unit (200), and the collection unit (100) includes a nozzle unit (110), a first pressure control unit (120), a solution storage unit (130), and a solution circulation unit (140), and the analysis unit (200) includes a sample storage unit (210), a second pressure control unit (220), and an analyzer (230), which are the same as the first and third embodiments.
[0142] The collection unit (100) is a component that collects an analysis sample by re-dissolving a thin film or pattern formed through a solution process and completing a residual solvent removal process.
[0143] The nozzle section (110) includes a discharge nozzle for discharging a standard reagent for dissolving a thin film or pattern to be collected, and a suction nozzle (114) for suctioning and recovering a solution redissolved by the discharged standard reagent.
[0144] In addition, the residual solvent analysis device through re-dissolution according to the sixth embodiment is the same as the third embodiment up to the structure in which a multi-needle type discharge nozzle (118) is applied to the nozzle section (110) of the collection section (100), but is different in that it further includes a saturated vapor pressure maintenance cover (300).
[0145] FIG. 9 is a drawing showing a configuration in which a saturated vapor pressure maintenance cover is added to the nozzle section of a residual solvent analysis device through redissolution according to the sixth embodiment of the present invention.
[0146] The nozzle section (110) of the residual solvent analysis device through re-dissolution according to the sixth embodiment further includes a saturated vapor pressure maintenance cover (300) that covers the upper portion of the position where re-dissolution and suction are performed by the multi-needle type discharge nozzle (118) and the suction nozzle (114), as shown.
[0147] The saturated vapor pressure maintenance cover (300) has a through hole (310) in the upper part into which a multi-needle type discharge nozzle (118) and a suction nozzle (114) are inserted, and is configured to cover the upper part and the side surface within a predetermined range where re-dissolution and suction are performed.
[0148] There is a problem that the re-dissolution efficiency decreases when the standard reagent discharged onto the thin film or pattern for re-dissolution evaporates, and the standard reagent may evaporate excessively due to mist, etc., which is generated because the standard reagent is discharged at a relatively high pressure. In particular, since the present embodiment requires minimizing the amount of standard reagent used in the process of obtaining the effect of concentrating the target substance by repeatedly using the standard reagent by applying the solution circulation unit (140), evaporation of the standard reagent may be a problem.
[0149] To solve this problem, in this embodiment, a saturated vapor pressure maintenance cover (300) is added, and evaporation of the standard reagent can be minimized by this saturated vapor pressure maintenance cover (300).
[0150] The first pressure control unit (120) is used to apply positive pressure during the process of discharging the standard reagent from the multi-needle type discharge nozzle (118) of the nozzle unit (110) and to apply negative pressure during the process of sucking the redissolved solution from the suction nozzle (114) of the nozzle unit (110).
[0151] In this embodiment, a thin film or pattern formed through a solution process and then subjected to a residual solvent removal process can be quickly re-dissolved and collected by suction through a multi-needle discharge nozzle (118) and a suction nozzle (114) connected to a first pressure control unit (120), so that a significant amount or the entire thin film or pattern formed on a substrate can be re-dissolved and inspected. Consequently, since more thin films or patterns can be re-dissolved and inspected for residual solvent with a similar amount of time and effort, the difficulty of the inspection can be lowered and the reliability of the inspection results can be improved.
[0152] The solution storage unit (130) includes a first reservoir (132) for storing a standard reagent to be discharged by a multi-needle type discharge nozzle (118) to re-dissolve a thin film or pattern formed by a solution process and proceeding to a residual solvent removal process, and a second reservoir (134) for sucking and storing a solution in which the thin film or pattern is re-dissolved by the discharged standard reagent.
[0153] The solution circulation unit (140) is equipped with a circulation line (142) and a circulation pump (144) to circulate the solution between the first reservoir (132) and the second reservoir (134).
[0154] The sample storage unit (210) stores test samples, etc. for performing tests on residual solvents. Since the concentration of the re-dissolved substance included in the test sample must be above a certain level in order to detect residual solvents, the concentration may be adjusted for the solution collected from the collection unit (100). However, as previously discussed, in the present embodiment, by applying the solution circulation unit (140) to the collection unit (100), a predetermined amount of standard reagent is repeatedly used for re-dissolution, so the concentration of the substance re-dissolved in the standard reagent continuously increases, and in most cases, the solution collected from the collection unit can be used as a test sample without a separate concentration process.
[0155] The second pressure control unit (220) is connected to apply positive or negative pressure to the sample storage unit (210), and the stored test sample can be transferred to the analyzer (230) using the positive pressure transmitted to the second pressure control unit (220).
[0156] The analyzer (230) is an analysis device that receives a test sample and analyzes the amount of residual solvent. A GC-MS analyzer may be used, but is not limited thereto.
[0157]
[0158] The present invention has been described above through preferred embodiments. However, the above-described embodiments are merely illustrative of the technical idea of the present invention. Those skilled in the art will understand that various changes may be made without departing from the technical idea of the present invention. Therefore, the scope of protection of the present invention should be interpreted not by specific embodiments, but by the matters described in the claims, and all technical ideas within a scope equivalent thereto should be interpreted as being included within the scope of the rights of the present invention.
Claims
1. A device for inspecting solvent remaining in a thin film or pattern formed through a solution process and undergoing a residual solvent removal process. A collection section for re-melting and collecting the thin film or pattern; and Includes an analysis unit that analyzes the collected test samples to test for residual solvents, The above extraction section, A nozzle unit including a discharge nozzle that discharges a standard reagent capable of dissolving a thin film or pattern and performing a residual solvent test, and a suction nozzle that collects a solution in which a thin film or pattern is dissolved by the standard reagent; A first pressure control unit for applying positive pressure to the discharge nozzle and negative pressure to the suction nozzle; A solution storage unit including a first reservoir for storing the solution discharged through the discharge nozzle and a second reservoir for storing the solution collected through the suction nozzle; and It includes a solution circulation unit that transfers and circulates the solution stored in the second reservoir to the first reservoir, The above analysis unit, A sample storage unit for storing test samples subject to residual solvent testing; and A residual solvent analysis device through redissolution, characterized by including an analyzer that receives a test sample stored in a sample storage unit and performs a residual solvent test.
2. In claim 1, A residual solvent analysis device through re-dissolution, characterized in that the above discharge nozzle is a needle-type discharge nozzle.
3. In claim 1, A residual solvent analysis device through re-dissolution, characterized in that the above discharge nozzle is a multi-needle type discharge nozzle.
4. In claim 1, A residual solvent analysis device through re-dissolution, characterized in that the first pressure control unit can generate positive pressure up to 500 kPa.
5. In claim 1, A residual solvent analysis device through re-dissolution, characterized in that the first pressure control unit can generate negative pressure of up to 50 kPa.
6. In claim 1, A residual solvent analysis device through redissolution, characterized in that the solution stored in the first reservoir is transferred to the sample storage unit by the positive pressure applied to the first reservoir.
7. In claim 1, The above analysis unit, A residual solvent analysis device through redissolution, characterized in that it includes a second pressure control unit that applies pressure to the sample storage unit.
8. In claim 7, A residual solvent analysis device through re-dissolution, characterized in that the second pressure control unit can generate a positive pressure of up to 100 kPa.
9. In claim 7, A residual solvent analysis device through re-dissolution, characterized in that the second pressure control unit can generate negative pressure of up to 10 kPa.
10. In claim 1, A residual solvent analysis device through redissolution, characterized in that the sample storage unit is connected to a syringe-type sample injection unit, and the analyzer has a syringe-type sample injection port.
11. In claim 1, A residual solvent analysis device through re-dissolution, characterized in that it further includes a moving device for moving the location of the sample storage unit.
12. In claim 1, A residual solvent analysis device through re-dissolution, characterized in that it further includes a saturated vapor pressure maintenance cover covering the upper portion of a position where re-dissolution and suction are performed by a discharge nozzle and a suction nozzle.
Citation Information
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