US20180292122A1 - System for trapping polymer vapors in process oven vacuum systems - Google Patents
System for trapping polymer vapors in process oven vacuum systems Download PDFInfo
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- US20180292122A1 US20180292122A1 US15/812,753 US201715812753A US2018292122A1 US 20180292122 A1 US20180292122 A1 US 20180292122A1 US 201715812753 A US201715812753 A US 201715812753A US 2018292122 A1 US2018292122 A1 US 2018292122A1
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- Prior art keywords
- trap assembly
- assembly
- polyimide
- trap
- vertical elevation
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Links
- 238000000034 method Methods 0.000 title claims abstract description 83
- 229920000642 polymer Polymers 0.000 title claims abstract description 19
- 229920001721 polyimide Polymers 0.000 claims abstract description 70
- 239000004642 Polyimide Substances 0.000 claims abstract description 68
- 238000009833 condensation Methods 0.000 claims abstract description 49
- 230000005494 condensation Effects 0.000 claims abstract description 49
- 238000001035 drying Methods 0.000 claims description 22
- 238000001816 cooling Methods 0.000 claims description 8
- 239000012530 fluid Substances 0.000 claims 27
- 239000007788 liquid Substances 0.000 abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 24
- 239000000758 substrate Substances 0.000 description 21
- 239000002243 precursor Substances 0.000 description 14
- 239000002904 solvent Substances 0.000 description 13
- 229910052757 nitrogen Inorganic materials 0.000 description 12
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 239000011261 inert gas Substances 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 6
- 239000007789 gas Substances 0.000 description 4
- 238000012423 maintenance Methods 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- 235000012431 wafers Nutrition 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000009719 polyimide resin Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000036760 body temperature Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000005587 bubbling Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229920000592 inorganic polymer Polymers 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000008450 motivation Effects 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0033—Other features
- B01D5/0045—Vacuum condensation
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25D—REFRIGERATORS; COLD ROOMS; ICE-BOXES; COOLING OR FREEZING APPARATUS NOT OTHERWISE PROVIDED FOR
- F25D21/00—Defrosting; Preventing frosting; Removing condensed or defrost water
- F25D21/14—Collecting or removing condensed and defrost water; Drip trays
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4487—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by using a condenser
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F04—POSITIVE - DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS FOR LIQUIDS OR ELASTIC FLUIDS
- F04B—POSITIVE-DISPLACEMENT MACHINES FOR LIQUIDS; PUMPS
- F04B37/00—Pumps having pertinent characteristics not provided for in, or of interest apart from, groups F04B25/00 - F04B35/00
- F04B37/10—Pumps having pertinent characteristics not provided for in, or of interest apart from, groups F04B25/00 - F04B35/00 for special use
- F04B37/14—Pumps having pertinent characteristics not provided for in, or of interest apart from, groups F04B25/00 - F04B35/00 for special use to obtain high vacuum
- F04B37/16—Means for nullifying unswept space
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25D—REFRIGERATORS; COLD ROOMS; ICE-BOXES; COOLING OR FREEZING APPARATUS NOT OTHERWISE PROVIDED FOR
- F25D19/00—Arrangement or mounting of refrigeration units with respect to devices or objects to be refrigerated, e.g. infrared detectors
Definitions
- This invention relates to vacuum systems, namely a system for trapping condensation in a designated location outside of a process oven.
- a continuing trend in semiconductor technology is the formation of integrated circuit (IC) chips having more and faster circuits thereon.
- IC integrated circuit
- Such ultralarge scale integration has resulted in a continued shrinkage of feature sizes with the result that a large number of devices are made available on a single chip.
- the interconnect density typically expands above the substrate in a multi-level arrangement and the devices have to be interconnected across these multiple levels.
- the interconnects must be electrically insulated from each other except where designed to make contact. Usually electrical insulation requires depositing dielectric films onto a surface, for example using a CVD or spinning-on process.
- the shrinkage in integrated circuit design rules has simultaneously reduced the wiring pitch. These have made the signal propagation delay in the interconnects an appreciable fraction of the total cycle time.
- low-k dielectric constant
- IC integrated circuit
- Polyimide is a polymer material often used in the production of semiconductor substrates such as silicon wafers.
- Polyimide is a desirable insulating material for semiconductor wafers because of its outstanding physical properties.
- polyimide typically requires a long time to cure when conventional heating techniques are used. A cure cycle of several hours is typical and this often becomes the pacing step in semiconductor fabrication.
- a polyimide precursor may be applied to a substrate, and then dried to prepare for imidization of the polymer.
- a goal of the drying process is to remove the solvent from the polymer (which may be N-Methyl-2-pyrrolidone, NMP, for example), and it can also be important to remove oxygen during the drying process.
- further goals of the drying process are to minimize or eliminate any bubbles/voids in the polymer layer, to minimize discoloration to the layer that may be induced by heating, and to fully remove residual solvent from the precursor mix. Each of these items sought to be eliminated may interfere with subsequent process steps, or enhance the probability of failure of a device containing the polyimide layer.
- Process ovens may be used to vacuum bake semiconductor substrates in support of various processes.
- a polyimide bake oven may be used for temperature imidization of polyimide layers, for example.
- Polymer vapors may be released during such processes, and these vapors would typically route through vacuum lines as part of their exit from the process chamber.
- a polyimide is temperature imidized at 400-450 C.
- a typical solvent for the process may be NMP. During the temperature imidization the vaporized solvents may carry vaporized polymer downstream, resulting in coating of the vacuum lines.
- the process may involve BCB and the temperature may be in the range of 350-400 C.
- the process may involve PBO and the temperature may be in the range of 200-250 C.
- the vacuum lines run the risk of having vaporized liquids condensing along their interiors, resulting in coatings within these lines. This may result in the need to replace these lines periodically, which may present quite a maintenance burden upon operators of such process ovens.
- Some process ovens incorporate filters into the vacuum systems, which are adapted to screen out the droplets in the vapor. This approach may still result in significant condensation within vacuum lines in the system.
- What is called for is a system which minimizes condensation in process ovens, and their fixed vacuum lines, and which collects condensed vapors in such a manner that allows for easy maintenance.
- FIGS. 1A and 1B are drawings of a process oven which may used in conjunction with embodiments of the present invention.
- FIG. 2 illustrates a trap assembly according to some embodiments of the present invention.
- FIG. 3 is a drawing of a trap assembly according to some embodiments of the present invention.
- FIG. 4 is a cutaway view of a trap assembly according to some embodiments of the present invention.
- FIG. 5 is an illustration of a cutaway view of a trap assembly according to some embodiments of the present invention.
- FIG. 6 is a colored view of a trap assembly on a bake oven according to some embodiments of the present invention.
- FIG. 7 is a colored view of a trap assembly on a bake oven according to some embodiments of the present invention.
- FIG. 8 is a colored cross-sectional view of a trap assembly on a bake oven according to some embodiments of the present invention.
- a trap system adapted to trap polyimide or other vapors exiting from a process chamber.
- the vapors are routed from the process chamber through a heated exit line at low pressure and then cooled, resulting in condensation at a selected location.
- the condensed vapors accumulate in a liquid trap.
- a polyimide bake oven 120 is coupled to a polyimide trap assembly 121 and is used to cure polyimide layers.
- the use of the polyimide bake oven 120 may involve heating of the oven in support of temperature imidization of a polymer layer while under vacuum, for example. These processes may also include drying of a polyimide precursor layer prior to the temperature imidization.
- the baking of the substrate with the polymer layer may release solvents during the heating/baking of the layer.
- the solvents may carry along with them some vaporized polymer, which presents the risk that the vaporized polymer may condense in places not desired.
- the vaporized polymer may condense in vacuum lines.
- the condensation within vacuum lines may decrease their functional capabilities as the cross-sectional flow area of the lines decrease with the polymer buildup along the interior walls of the lines.
- the polyimide bake oven 120 may include a main chamber 125 and a feeder assembly 126 .
- the feeder assembly 126 may allow for the insertion into the polyimide bake oven 120 of stacks of horizontally laid wafers.
- the polyimide trap assembly 121 may include a trap assembly inlet 133 that is coupled to a vacuum exit line 132 from the main chamber 125 .
- the vacuum exit line 132 may be heated with a heater 130 in order to minimize condensation within the line.
- a thermocouple 131 may be present on the vacuum exit line 132 . With a heated process oven, and then a heated vacuum exit line 132 , the amount of condensation within the process oven and the heated vacuum exit line 132 may be kept to a minimum.
- the vacuum exit line 132 may have a cross-sectional flow area of a first amount.
- the polyimide trap assembly 121 is adapted to cause condensation of the polymer vapor flowing in the vacuum line in a specific location, so that the condensation does not occur in other portions of the system. Without such a system, it is expected that the exhaust piping will be impacted the further it is from the main chamber. As the exhausted vapor leaves the main chamber, it may remain as vapor at the exit temperature. Farther along a globular polyimide will form in the piping, and then farther along a coating will form. This will interfere with exhaust flow. With enough time the piping will become sufficiently, or completely, blocked which then requires removal and replacement of components. With the polyimide trap assembly the condensation may be so complete at the trap that no further downstream condensate forms, sparing the operator from costly and time consuming maintenance.
- the trap inlet 133 routes the chamber exhaust into a condensing body 122 .
- the condensing body 122 may be of aluminum and have fins 137 which allow for heat transfer from the hot chamber exhaust to the outside environment.
- a trap cooling blower 123 is coupled to the condensing body 122 .
- Auxiliary fans 124 may further provide air to recirculate the area around the condensing body.
- the exhaust travels out of the condensing body 122 through the trap outlet 136 .
- the condensed liquid flows downward into the vial 134 .
- the vial 134 may be clear and may be of glass.
- a clamp assembly 135 may include a clamp and an 0 -ring seal.
- the amount of liquid in the vial 134 may be observed by the operator.
- the operator may remove and replace the vial with a new or emptied vial.
- condensation of the polyimide now restricted to a chosen location and the condensed polyimide routed to the vial 134
- replacement of the vial 134 is the only process step needed to remove condensed polyimide.
- other portions of the polyimide bake oven 120 and its exhaust and vacuum system are protected from condensation of polyimide, which previously required time consuming maintenance for its removal.
- the vacuum trap system is thus geared to control the location where condensation of polymer vapors is likely to occur.
- FIGS. 5 and 8 are cross-sectional views of a trap assembly according to some embodiments of the present invention.
- FIGS. 6 and 7 are illustrations of a bake oven with a trap assembly according to some embodiments of the present invention.
- a drying process is carried out in a process chamber with low pressure/vacuum capabilities.
- the process chamber may also include capability for inletting heated inert gas, such as nitrogen.
- the process chamber may also be able to be heated for supporting the drying process.
- the process chamber may also be able to be heated to even higher temperatures to support temperature imidization processing after the drying portion of the process.
- the process chamber is coupled to a polyimide trap assembly as discussed aboe.
- the solvent With reduced pressure, the solvent will boil at a lower temperature. For example, NMP boils at approximately 105 C at 50 Torr.
- the substrates are delivered into a process chamber.
- the process chamber may be heated to a temperature below the room temperature boiling point of the solvent.
- the solvent may be NMP and the initial heating temperature may be 150 C.
- the pressure used is subject to at least two conflicting constraints. On the one hand, the pressure should be reduced enough to evaporate the solvent, allowing for the low pressure liberation of the gas which permeates the liquid/gel precursor and is liberated to the low pressure chamber.
- a polyimide precursor is applied to a silicon substrate.
- the polyimide precursor is applied directly over the silicon substrate.
- the polyimide precursor is applied over other layers already on a substrate, which may be other polyimide layers and metal layers, for example.
- the solvent used in the polyimide precursor is NMP.
- An expected thickness for semiconductor applications is in the range of 7-10 microns.
- a process oven may be used to support a plurality of substrates within a chamber .
- the process oven may include internal heaters, heated inert gas inputs, and vacuum capability.
- the substrates are placed into the chamber that has been heated to 150 C.
- the chamber is heated to a temperature in the range of 135 C to 180 C.
- the chamber pressure is reduced to a first drying pressure of 50 Torr.
- the first drying pressure is in the range of 30-60 Torr.
- the chamber may then be flushed with a heated inert gas such as nitrogen at a pressure of 600 Torr.
- the heated inert gas may be at a pressure in the range of 550 to 760 Torr.
- the nitrogen may be heated to the same temperature as the chamber, 150 C.
- the chamber pressure is then reduced to a second drying pressure of 25 Torr.
- the second drying pressure is in the range of 15-30 Torr.
- the chamber may then be flushed with a heated inert gas such as nitrogen at a pressure of 600 Torr.
- the heated inert gas may be at a pressure in the range of 550 to 760 Torr.
- the nitrogen may be heated to the same temperature as the chamber, 150 C.
- the chamber pressure is then reduced to a third drying temperature of 1 Torr. In some embodiments, the third drying pressure is in the range of 1-15 Torr.
- the chamber may then be filled with heated inert gas, such as nitrogen, up to 650 Torr, in preparation for imidization of the polyimide precursor.
- heated inert gas such as nitrogen, up to 650 Torr
- the substrates may then undergo temperature imidization in the same chamber.
- the subsequent temperature imidization may occur at 350-375 C, and as further described below.
- Each of these process steps may liberate process affluent laden with polyimide vapor, which may clog the vacuum exhaust system downstream from the process chamber.
- a process may begin with the heating of the process oven to a temperature of 150 C.
- a single substrate or a plurality of substrates within the process oven which include a polyimide precursor including a solvent such as MP, are put into the process oven which has been preheated to the temperature of 150 C.
- the process oven pressure is then reduced to a first drying pressure of 50 Torr. This portion of the process may take 2-3 minutes.
- the process oven is then flushed with preheated nitrogen heated to 150 C up to a pressure of 600 Torr. This portion of the process may take 2-3 minutes.
- the process oven pressure is then reduced to a second drying pressure of 25 Torr. This portion of the process may take 3-4 minutes.
- the process oven is then flushed with preheated nitrogen heated to 150 C up to a pressure of 600 Torr. This portion of the process may take 2-3 minutes.
- the process oven pressure is then reduced to a third drying pressure of 1 Torr. This portion of the process may take 4-5 minutes.
- the process oven is then flushed with preheated nitrogen heated to 150 C up to a pressure of 650 Torr. This portion of the process may take 2-3 minutes.
- the aforementioned steps have now greatly reduced the oxygen level in the process oven, as well as having removed all or nearly all of the solvent from the polyimide precursor with little or no bubbling or skinning of the polyimide precursor.
- the substrates are now ready for temperature imidization.
- the oxygen level in the process oven may now be down as low as approximately 1 ppm, as an end result of the drying process.
- An exemplary temperature imidization process may now include maintaining approximately 250 Torr in the process chamber while inputting heated nitrogen at the top of the process oven while pulling vacuum at the bottom of the process oven.
- the heated nitrogen and the oven temperatures may now be raised in unison, for example, to 350 C. At 4 C/minute, this heating process would take 50 minutes.
- 350 C the oven and gas temperatures may be held for 1 hour for temperature imidization of the polyimide precursor.
- 350 C is an illustrative temperature using NMP, other temperatures may be used for the temperature imidization.
- affluent laden with polyimide vapor may be liberated from the polyimide layers on the substrates.
- the process step of maintaining a pressure, such as 250 Torr, while curing the polyimide may result in a continuous flow of process affluent through the vacuum outlet.
- the vacuum outlet system and its piping were subject to clogging by the condensation of the polyimide in the system and piping.
- the use of the polyimide trap assembly as described above allows for the location of the polyimide condensation to be determined, and for the trapping of the polyimide condensation in a reservoir which his easily removable and replaceable.
- the oven heaters may be turned off, which will result in a cooling of the oven.
- the heated nitrogen flow may be cooled at a rate which tracks the cooling oven.
- the length of the vacuum exit line may be varied such that the flow through the line is cooled enough to allow for complete or near complete condensation in the condensation chamber.
- the length of the vacuum exit line may be selected such that the vacuum exit line is not subject to clogging condensation.
- the length of the vacuum exit line may be varied depending upon the temperature used in the oven, the polyimide type used in the oven during processing, and other factors. In one example, the temperature of the vacuum exit line at the entrance to the condensation body was approximately 65 C, the cooled condensation body temperature was approximately 30 C, and the condensation body exit line was approximately 44 C.
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Abstract
Description
- This application claims priority to U.S. Provisional Patent Application No. 62/421,671 to Moffat et al., filed Nov. 14, 2017, which is hereby incorporated by reference in its entirety.
- This invention relates to vacuum systems, namely a system for trapping condensation in a designated location outside of a process oven.
- A continuing trend in semiconductor technology is the formation of integrated circuit (IC) chips having more and faster circuits thereon. Such ultralarge scale integration has resulted in a continued shrinkage of feature sizes with the result that a large number of devices are made available on a single chip. With a limited chip surface area, the interconnect density typically expands above the substrate in a multi-level arrangement and the devices have to be interconnected across these multiple levels. The interconnects must be electrically insulated from each other except where designed to make contact. Usually electrical insulation requires depositing dielectric films onto a surface, for example using a CVD or spinning-on process. The shrinkage in integrated circuit design rules has simultaneously reduced the wiring pitch. These have made the signal propagation delay in the interconnects an appreciable fraction of the total cycle time. The motivation to minimize signal delay has driven extensive studies to develop a low dielectric constant (low-k) material that can be used as an inter-level dielectric in integrated circuit (IC) manufacturing. The majority of low-k materials used in the ILD layer are based on thermally cured spin-on organic or inorganic polymers.
- Polyimide is a polymer material often used in the production of semiconductor substrates such as silicon wafers. Polyimide is a desirable insulating material for semiconductor wafers because of its outstanding physical properties. Unfortunately, polyimide typically requires a long time to cure when conventional heating techniques are used. A cure cycle of several hours is typical and this often becomes the pacing step in semiconductor fabrication. In addition, there are other problems involved with curing polyimide resin with conventional heat. For example, when polyimide resin is cured in a conventional furnace, the outer surface of the resin typically cures faster than the center portions. This can cause various physical defects, such as the formation of voids, and can result in inferior mechanical properties such as reduced modulus, enhanced swelling, solvent uptake, and coefficient of thermal expansion.
- A polyimide precursor may be applied to a substrate, and then dried to prepare for imidization of the polymer. A goal of the drying process is to remove the solvent from the polymer (which may be N-Methyl-2-pyrrolidone, NMP, for example), and it can also be important to remove oxygen during the drying process. In addition, further goals of the drying process are to minimize or eliminate any bubbles/voids in the polymer layer, to minimize discoloration to the layer that may be induced by heating, and to fully remove residual solvent from the precursor mix. Each of these items sought to be eliminated may interfere with subsequent process steps, or enhance the probability of failure of a device containing the polyimide layer.
- Process ovens may be used to vacuum bake semiconductor substrates in support of various processes. A polyimide bake oven may be used for temperature imidization of polyimide layers, for example. Polymer vapors may be released during such processes, and these vapors would typically route through vacuum lines as part of their exit from the process chamber.
- In some such processes, a polyimide is temperature imidized at 400-450 C. A typical solvent for the process may be NMP. During the temperature imidization the vaporized solvents may carry vaporized polymer downstream, resulting in coating of the vacuum lines. In another exemplary process, the process may involve BCB and the temperature may be in the range of 350-400 C. In another exemplary process, the process may involve PBO and the temperature may be in the range of 200-250 C.
- The vacuum lines run the risk of having vaporized liquids condensing along their interiors, resulting in coatings within these lines. This may result in the need to replace these lines periodically, which may present quite a maintenance burden upon operators of such process ovens. Some process ovens incorporate filters into the vacuum systems, which are adapted to screen out the droplets in the vapor. This approach may still result in significant condensation within vacuum lines in the system.
- What is called for is a system which minimizes condensation in process ovens, and their fixed vacuum lines, and which collects condensed vapors in such a manner that allows for easy maintenance.
-
FIGS. 1A and 1B are drawings of a process oven which may used in conjunction with embodiments of the present invention. -
FIG. 2 illustrates a trap assembly according to some embodiments of the present invention. -
FIG. 3 is a drawing of a trap assembly according to some embodiments of the present invention. -
FIG. 4 is a cutaway view of a trap assembly according to some embodiments of the present invention. -
FIG. 5 is an illustration of a cutaway view of a trap assembly according to some embodiments of the present invention. -
FIG. 6 is a colored view of a trap assembly on a bake oven according to some embodiments of the present invention. -
FIG. 7 is a colored view of a trap assembly on a bake oven according to some embodiments of the present invention. -
FIG. 8 is a colored cross-sectional view of a trap assembly on a bake oven according to some embodiments of the present invention. - A trap system adapted to trap polyimide or other vapors exiting from a process chamber. The vapors are routed from the process chamber through a heated exit line at low pressure and then cooled, resulting in condensation at a selected location. The condensed vapors accumulate in a liquid trap. A method of condensing polymer vapors in vacuum exit lines of process chambers, where the flow which may have vaporized polymer vapor is cooled to enhance condensation at a chosen location.
- In some embodiments of the present invention, as seen in
FIGS. 1A and 1B , apolyimide bake oven 120 is coupled to apolyimide trap assembly 121 and is used to cure polyimide layers. The use of thepolyimide bake oven 120 may involve heating of the oven in support of temperature imidization of a polymer layer while under vacuum, for example. These processes may also include drying of a polyimide precursor layer prior to the temperature imidization. The baking of the substrate with the polymer layer may release solvents during the heating/baking of the layer. The solvents may carry along with them some vaporized polymer, which presents the risk that the vaporized polymer may condense in places not desired. For example, the vaporized polymer may condense in vacuum lines. The condensation within vacuum lines may decrease their functional capabilities as the cross-sectional flow area of the lines decrease with the polymer buildup along the interior walls of the lines. - The
polyimide bake oven 120 may include amain chamber 125 and afeeder assembly 126. Thefeeder assembly 126 may allow for the insertion into thepolyimide bake oven 120 of stacks of horizontally laid wafers. - The polyimide trap assembly 121may include a
trap assembly inlet 133 that is coupled to avacuum exit line 132 from themain chamber 125. Thevacuum exit line 132 may be heated with aheater 130 in order to minimize condensation within the line. Athermocouple 131 may be present on thevacuum exit line 132. With a heated process oven, and then a heatedvacuum exit line 132, the amount of condensation within the process oven and the heatedvacuum exit line 132 may be kept to a minimum. Thevacuum exit line 132 may have a cross-sectional flow area of a first amount. - As the exhausting vapors travel further from the main chamber, they enter a
polyimide trap assembly 121 which cools the flowing vapors, leading to condensation. Thepolyimide trap assembly 121 is adapted to cause condensation of the polymer vapor flowing in the vacuum line in a specific location, so that the condensation does not occur in other portions of the system. Without such a system, it is expected that the exhaust piping will be impacted the further it is from the main chamber. As the exhausted vapor leaves the main chamber, it may remain as vapor at the exit temperature. Farther along a globular polyimide will form in the piping, and then farther along a coating will form. This will interfere with exhaust flow. With enough time the piping will become sufficiently, or completely, blocked which then requires removal and replacement of components. With the polyimide trap assembly the condensation may be so complete at the trap that no further downstream condensate forms, sparing the operator from costly and time consuming maintenance. - As also seen in
FIGS. 2, 3, and 4 , thetrap inlet 133 routes the chamber exhaust into a condensingbody 122. The condensingbody 122 may be of aluminum and havefins 137 which allow for heat transfer from the hot chamber exhaust to the outside environment. Atrap cooling blower 123 is coupled to the condensingbody 122. As the exhaust passes into theinterior space 138 the exhaust is cooled, which allows for condensation of the vaporized polyimide into liquid which then flows 139 downward assisted by gravity.Auxiliary fans 124 may further provide air to recirculate the area around the condensing body. The exhaust travels out of the condensingbody 122 through thetrap outlet 136. The condensed liquid flows downward into thevial 134. Thevial 134 may be clear and may be of glass. Aclamp assembly 135 may include a clamp and an 0-ring seal. - In practice, the amount of liquid in the
vial 134 may be observed by the operator. When the liquid is starting to fill thevial 134, the operator may remove and replace the vial with a new or emptied vial. With condensation of the polyimide now restricted to a chosen location and the condensed polyimide routed to thevial 134, replacement of thevial 134 is the only process step needed to remove condensed polyimide. Further, other portions of thepolyimide bake oven 120 and its exhaust and vacuum system are protected from condensation of polyimide, which previously required time consuming maintenance for its removal. The vacuum trap system is thus geared to control the location where condensation of polymer vapors is likely to occur. -
FIGS. 5 and 8 are cross-sectional views of a trap assembly according to some embodiments of the present invention.FIGS. 6 and 7 are illustrations of a bake oven with a trap assembly according to some embodiments of the present invention. - In some embodiments of the present invention, a drying process is carried out in a process chamber with low pressure/vacuum capabilities. The process chamber may also include capability for inletting heated inert gas, such as nitrogen. The process chamber may also be able to be heated for supporting the drying process. The process chamber may also be able to be heated to even higher temperatures to support temperature imidization processing after the drying portion of the process. The process chamber is coupled to a polyimide trap assembly as discussed aboe.
- With reduced pressure, the solvent will boil at a lower temperature. For example, NMP boils at approximately 105 C at 50 Torr. Using an example of a substrate coated with a polyimide precursor, or a plurality of such coated substrates, the substrates are delivered into a process chamber. The process chamber may be heated to a temperature below the room temperature boiling point of the solvent. The solvent may be NMP and the initial heating temperature may be 150 C. The pressure used is subject to at least two conflicting constraints. On the one hand, the pressure should be reduced enough to evaporate the solvent, allowing for the low pressure liberation of the gas which permeates the liquid/gel precursor and is liberated to the low pressure chamber. On the other hand, too much evaporation, too quickly, could lead to aggregation of the gas into bubbles, which may lead to popping on the surface or other issues. Further, though, lowering the chamber pressure in further steps to a pressure even lower than 50 Torr creates more pressure differential between the bottom of the gel, against the substrate, and the low pressure chamber, better driving out the gas.
- In an exemplary process according to some embodiments of the present invention, a polyimide precursor is applied to a silicon substrate. In some aspects, the polyimide precursor is applied directly over the silicon substrate. In some aspects, the polyimide precursor is applied over other layers already on a substrate, which may be other polyimide layers and metal layers, for example. In some aspects, the solvent used in the polyimide precursor is NMP. An expected thickness for semiconductor applications is in the range of 7-10 microns. Although a single substrate could be processed, in some aspects a plurality of substrates may be processed.
- A process oven may be used to support a plurality of substrates within a chamber . The process oven may include internal heaters, heated inert gas inputs, and vacuum capability. In an exemplary embodiment, the substrates are placed into the chamber that has been heated to 150 C. In some aspects, the chamber is heated to a temperature in the range of 135 C to 180 C. The chamber pressure is reduced to a first drying pressure of 50 Torr. In some embodiments, the first drying pressure is in the range of 30-60 Torr. After reaching the first drying pressure, the chamber may then be flushed with a heated inert gas such as nitrogen at a pressure of 600 Torr. In some aspects the heated inert gas may be at a pressure in the range of 550 to 760 Torr. The nitrogen may be heated to the same temperature as the chamber, 150 C. The chamber pressure is then reduced to a second drying pressure of 25 Torr. In some embodiments, the second drying pressure is in the range of 15-30 Torr. After reaching the second drying pressure, the chamber may then be flushed with a heated inert gas such as nitrogen at a pressure of 600 Torr. In some aspects the heated inert gas may be at a pressure in the range of 550 to 760 Torr. The nitrogen may be heated to the same temperature as the chamber, 150 C. The chamber pressure is then reduced to a third drying temperature of 1 Torr. In some embodiments, the third drying pressure is in the range of 1-15 Torr. After reaching the third drying pressure, the chamber may then be filled with heated inert gas, such as nitrogen, up to 650 Torr, in preparation for imidization of the polyimide precursor. The substrates may then undergo temperature imidization in the same chamber. The subsequent temperature imidization may occur at 350-375 C, and as further described below. Each of these process steps may liberate process affluent laden with polyimide vapor, which may clog the vacuum exhaust system downstream from the process chamber.
- In an exemplary embodiment further illustrating the timing of a process as described above, a process may begin with the heating of the process oven to a temperature of 150 C. A single substrate or a plurality of substrates within the process oven, which include a polyimide precursor including a solvent such as MP, are put into the process oven which has been preheated to the temperature of 150 C. The process oven pressure is then reduced to a first drying pressure of 50 Torr. This portion of the process may take 2-3 minutes. The process oven is then flushed with preheated nitrogen heated to 150 C up to a pressure of 600 Torr. This portion of the process may take 2-3 minutes. The process oven pressure is then reduced to a second drying pressure of 25 Torr. This portion of the process may take 3-4 minutes. The process oven is then flushed with preheated nitrogen heated to 150 C up to a pressure of 600 Torr. This portion of the process may take 2-3 minutes. The process oven pressure is then reduced to a third drying pressure of 1 Torr. This portion of the process may take 4-5 minutes. The process oven is then flushed with preheated nitrogen heated to 150 C up to a pressure of 650 Torr. This portion of the process may take 2-3 minutes. The aforementioned steps have now greatly reduced the oxygen level in the process oven, as well as having removed all or nearly all of the solvent from the polyimide precursor with little or no bubbling or skinning of the polyimide precursor.
- After the multi-step drying process, the substrates are now ready for temperature imidization. As discussed further below, the oxygen level in the process oven may now be down as low as approximately 1 ppm, as an end result of the drying process. An exemplary temperature imidization process may now include maintaining approximately 250 Torr in the process chamber while inputting heated nitrogen at the top of the process oven while pulling vacuum at the bottom of the process oven. The heated nitrogen and the oven temperatures may now be raised in unison, for example, to 350 C. At 4 C/minute, this heating process would take 50 minutes. At 350 C the oven and gas temperatures may be held for 1 hour for temperature imidization of the polyimide precursor. Although 350 C is an illustrative temperature using NMP, other temperatures may be used for the temperature imidization. During the temperature imidization process affluent laden with polyimide vapor may be liberated from the polyimide layers on the substrates. The process step of maintaining a pressure, such as 250 Torr, while curing the polyimide may result in a continuous flow of process affluent through the vacuum outlet. In prior applications, the vacuum outlet system and its piping were subject to clogging by the condensation of the polyimide in the system and piping. The use of the polyimide trap assembly as described above allows for the location of the polyimide condensation to be determined, and for the trapping of the polyimide condensation in a reservoir which his easily removable and replaceable. After the temperature imidization, the oven heaters may be turned off, which will result in a cooling of the oven. The heated nitrogen flow may be cooled at a rate which tracks the cooling oven.
- In some aspects, the length of the vacuum exit line may be varied such that the flow through the line is cooled enough to allow for complete or near complete condensation in the condensation chamber. The length of the vacuum exit line may be selected such that the vacuum exit line is not subject to clogging condensation. The length of the vacuum exit line may be varied depending upon the temperature used in the oven, the polyimide type used in the oven during processing, and other factors. In one example, the temperature of the vacuum exit line at the entrance to the condensation body was approximately 65 C, the cooled condensation body temperature was approximately 30 C, and the condensation body exit line was approximately 44 C.
- As evident from the above description, a wide variety of embodiments may be configured from the description given herein and additional advantages and modifications will readily occur to those skilled in the art. The invention in its broader aspects is, therefore, not limited to the specific details and illustrative examples shown and described. Accordingly, departures from such details may be made without departing from the spirit or scope of the applicant's general invention.
Claims (33)
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
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US15/812,753 US20180292122A1 (en) | 2016-11-14 | 2017-11-14 | System for trapping polymer vapors in process oven vacuum systems |
PCT/US2018/060814 WO2019099401A2 (en) | 2016-11-14 | 2018-11-13 | Trap assembly and system for trapping polymer vapors in process oven vacuum systems |
US16/189,631 US20190314738A1 (en) | 2016-11-14 | 2018-11-13 | Trap assembly and system for trapping polymer vapors in process oven vacuum systems |
TW107140455A TW201924761A (en) | 2016-11-14 | 2018-11-14 | Trap assembly and system for trapping polymer vapors in process oven vacuum systems |
Applications Claiming Priority (2)
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US201662421671P | 2016-11-14 | 2016-11-14 | |
US15/812,753 US20180292122A1 (en) | 2016-11-14 | 2017-11-14 | System for trapping polymer vapors in process oven vacuum systems |
Related Child Applications (1)
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US16/189,631 Continuation-In-Part US20190314738A1 (en) | 2016-11-14 | 2018-11-13 | Trap assembly and system for trapping polymer vapors in process oven vacuum systems |
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US20180292122A1 true US20180292122A1 (en) | 2018-10-11 |
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US15/812,753 Abandoned US20180292122A1 (en) | 2016-11-14 | 2017-11-14 | System for trapping polymer vapors in process oven vacuum systems |
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US (1) | US20180292122A1 (en) |
TW (1) | TW201924761A (en) |
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WO2024011677A1 (en) * | 2022-07-14 | 2024-01-18 | 长鑫存储技术有限公司 | Semiconductor processing device, waste gas treatment mechanism, and method |
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CN110064262A (en) * | 2019-05-16 | 2019-07-30 | 深圳市中科智诚科技有限公司 | A kind of coal chemical industry wet-scrubbing equipment with dredging function of good dedusting effect |
US11444053B2 (en) | 2020-02-25 | 2022-09-13 | Yield Engineering Systems, Inc. | Batch processing oven and method |
US11688621B2 (en) | 2020-12-10 | 2023-06-27 | Yield Engineering Systems, Inc. | Batch processing oven and operating methods |
CN117488274B (en) * | 2023-12-28 | 2024-03-26 | 杭州嘉悦智能设备有限公司 | Condensation collection structure and silicon oxide production equipment |
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Also Published As
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WO2018090048A1 (en) | 2018-05-17 |
WO2019099401A2 (en) | 2019-05-23 |
TW201924761A (en) | 2019-07-01 |
WO2019099401A3 (en) | 2019-10-17 |
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