WO2009119343A1 - 表面処理装置、及び表面処理方法 - Google Patents
表面処理装置、及び表面処理方法 Download PDFInfo
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- WO2009119343A1 WO2009119343A1 PCT/JP2009/054885 JP2009054885W WO2009119343A1 WO 2009119343 A1 WO2009119343 A1 WO 2009119343A1 JP 2009054885 W JP2009054885 W JP 2009054885W WO 2009119343 A1 WO2009119343 A1 WO 2009119343A1
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- Prior art keywords
- adhesion promoter
- substrate
- holding
- vapor
- water
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- 238000000034 method Methods 0.000 title claims description 44
- 239000002318 adhesion promoter Substances 0.000 claims abstract description 158
- 239000000758 substrate Substances 0.000 claims abstract description 144
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 79
- 238000010438 heat treatment Methods 0.000 claims abstract description 37
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 32
- 239000007864 aqueous solution Substances 0.000 claims abstract description 28
- 230000008016 vaporization Effects 0.000 claims description 48
- 238000012545 processing Methods 0.000 claims description 41
- 238000004381 surface treatment Methods 0.000 claims description 37
- 239000011550 stock solution Substances 0.000 claims description 23
- 238000009834 vaporization Methods 0.000 claims description 20
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 18
- 230000018044 dehydration Effects 0.000 claims description 15
- 238000002156 mixing Methods 0.000 claims description 8
- 230000008021 deposition Effects 0.000 claims 1
- 239000010408 film Substances 0.000 description 113
- 229920000642 polymer Polymers 0.000 description 46
- 125000000524 functional group Chemical group 0.000 description 15
- 238000006460 hydrolysis reaction Methods 0.000 description 15
- 230000015572 biosynthetic process Effects 0.000 description 14
- 239000000178 monomer Substances 0.000 description 11
- 238000010586 diagram Methods 0.000 description 10
- 239000002994 raw material Substances 0.000 description 10
- 230000007062 hydrolysis Effects 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000006116 polymerization reaction Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 239000000853 adhesive Substances 0.000 description 5
- 230000001070 adhesive effect Effects 0.000 description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 5
- 229920001721 polyimide Polymers 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 230000009257 reactivity Effects 0.000 description 5
- 230000007246 mechanism Effects 0.000 description 4
- 238000003672 processing method Methods 0.000 description 4
- 238000012719 thermal polymerization Methods 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 238000007740 vapor deposition Methods 0.000 description 4
- 238000006482 condensation reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
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- 206010037660 Pyrexia Diseases 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
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- 238000004519 manufacturing process Methods 0.000 description 2
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- 238000012986 modification Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004642 Polyimide Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
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- 229910052760 oxygen Inorganic materials 0.000 description 1
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Images
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
- H01L21/312—Organic layers, e.g. photoresist
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02109—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates
- H01L21/02112—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer
- H01L21/02123—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon
- H01L21/02126—Forming insulating materials on a substrate characterised by the type of layer, e.g. type of material, porous/non-porous, pre-cursors, mixtures or laminates characterised by the material of the layer the material containing silicon the material containing Si, O, and at least one of H, N, C, F, or other non-metal elements, e.g. SiOC, SiOC:H or SiONC
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D1/00—Processes for applying liquids or other fluent materials
- B05D1/60—Deposition of organic layers from vapour phase
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02296—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer
- H01L21/02299—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer pre-treatment
- H01L21/02312—Forming insulating materials on a substrate characterised by the treatment performed before or after the formation of the layer pre-treatment treatment by exposure to a gas or vapour
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/007—After-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/10—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an adhesive surface
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
- H01L21/02107—Forming insulating materials on a substrate
- H01L21/02225—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer
- H01L21/0226—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process
- H01L21/02282—Forming insulating materials on a substrate characterised by the process for the formation of the insulating layer formation by a deposition process liquid deposition, e.g. spin-coating, sol-gel techniques, spray coating
Definitions
- the present invention relates to a substrate surface treatment apparatus and a substrate surface treatment method, and more particularly to a substrate surface treatment apparatus and a substrate surface treatment method suitable for forming an organic film through a thermal polymerization reaction.
- the present invention also relates to a film forming apparatus and a film forming method using the surface treatment apparatus and the surface treatment method.
- a polymer organic film is useful as an interlayer insulating film such as LSI or a liquid crystal alignment film, and has very excellent electrical, optical, and mechanical properties.
- polyimide for example, has a high glass transition point and is excellent in heat resistance, chemical stability, orientation controllability, etc., so it is also used as a heat-resistant radiation material, space material, and a superconducting magnet used in a nuclear fusion reactor. It is also considered to use it as an insulating material or a protective material that prevents deterioration of equipment due to atomic oxygen in outer space.
- a vapor deposition polymerization method vacuum vapor deposition polymerization method
- raw material monomers are evaporated in a vacuum chamber and polymerized on a substrate to directly obtain an organic film. Since this method is a dry process and is a process under non-thermal equilibrium, an organic film that cannot be obtained by a conventional chemical wet process can be obtained. In this method, since the raw material monomer enters and adheres to the unevenness of the substrate, it is possible to perform film formation with good coverage (Patent Document 1).
- the adhesion between the polymer organic film and the substrate is low, and particularly when a semiconductor substrate is used as the substrate, the adhesion tends to be remarkably deteriorated.
- an aqueous solution containing an adhesion promoter such as a silane coupling agent is prepared, the substrate is immersed in the solution, and the adhesion promoter is adhered on the surface of the substrate, and the adhesion Attempts have been made to improve the adhesion between the substrate and the polymer organic film through an accelerator.
- an adhesion promoter such as a silane coupling agent
- the adhesion promoter aqueous solution is first applied on the surface of the substrate, and then the applied aqueous solution is dried to allow only the adhesion promoter to be the substrate. To remain on the surface.
- the residue may adversely affect the polymer organic film.
- Patent Document 2 a silane coupling agent is introduced as a vapor into a processing vessel, and the silane coupling agent vapor is adhered onto the surface of the substrate, and the residue resulting from the above-described liquid pool is removed.
- a method for suppressing the occurrence is disclosed.
- this method has a problem in that the adhesion between the substrate and the polymer organic film formed thereafter is not sufficiently improved.
- an object of the present invention is to improve adhesion between a substrate, particularly a semiconductor substrate and a polymer organic film, without generating a residue due to an adhesion promoter on the substrate.
- the present invention provides: A holding container for an aqueous solution containing 20% by volume or more of an adhesion promoter; A heater for vaporization for heating and vaporizing the aqueous solution in the holding container at a temperature of 80 to 100 ° C. to generate a water-containing adhesion promoter vapor; After the water-containing adhesion promoter vapor adheres and condenses on the surface of the substrate, a heating dehydration heater that causes a heat dehydration reaction to chemically bond the adhesion promoter to the surface of the substrate; A processing container for storing at least the holding container and holding the adhesion promoter vapor; And a substrate surface processing apparatus (first processing apparatus).
- the present invention also provides: A first holding container for holding a stock solution of an adhesion promoter; A second holding container for holding water; A first vaporizing heater for heating and vaporizing the stock solution of the adhesion promoter in the first holding container to generate an adhesion promoter vapor; A second vaporization heater for heating and vaporizing the water in the second holding container to generate water vapor; Heat dehydration in which the adhesion promoter vapor and the water vapor in which the adhesion promoter is maintained at a predetermined mixing ratio or more on the surface of the substrate adheres and hydrolyzes, and then the adhesion promoter is chemically bonded to the surface of the substrate.
- the present invention provides: Holding an aqueous solution containing an adhesion promoter of 20% by volume or more in a holding container; Heating and vaporizing the aqueous solution to a temperature of 80 to 100 ° C. with a vaporizing heater to generate a water-containing adhesion promoter vapor and holding it in a processing vessel; A step of causing the water-containing adhesion promoter vapor to adhere to and condense on the surface of the substrate, causing a heat dehydration reaction with a heater for heat dehydration, and dehydrating and condensing the adhesion promoter on the surface of the substrate; And a substrate surface treatment method (first treatment method).
- the present invention also provides: Holding the stock solution of the adhesion promoter in the first holding container; Holding water in a second holding container; Heating and vaporizing the adhesion promoter stock solution in the first holding container with a first vaporization heater to generate an adhesion promoter vapor and holding it in the processing container; Heating and vaporizing the water in the second holding container with a second vaporizing heater to generate water vapor, and holding the water in the processing container; After the adhesion promoter vapor and the water vapor in which the adhesion promoter is maintained at a predetermined mixing ratio or more adhere to the surface of the substrate and hydrolyze, it is dehydrated and condensed with a heater for heating and dehydration, and is applied to the surface of the substrate. Chemically bonding the adhesion promoter; And a substrate surface treatment method (second treatment method).
- the adhesion promoter is attached not as a solution but as a vapor to the surface of the substrate, it is possible to suppress the generation of a residue due to the liquid pool resulting from the solution application. . Therefore, the residue does not adversely affect the polymer organic film formed on the substrate surface thereafter, and the characteristics thereof are not deteriorated.
- an aqueous solution containing the adhesion promoter is prepared in advance, and the aqueous solution is heated and vaporized.
- the adhesion promoter and water vapor are included. Therefore, the adhesion promoter is attached to the surface of the substrate. Therefore, the adhesion promoter and water react with each other on the surface, and a reactive functional group is exposed on the surface of the adhesion promoter.
- the vapor is attached and aggregated on the surface of the substrate, and then heat treatment is performed.
- the adhesion promoter is dehydrated and condensed, and the functional groups exposed on the surface of the adhesion promoter react with the surface of the substrate. Accordingly, the adhesion between the adhesion promoter and the substrate is improved.
- the adhesion between the adhesion promoter and the polymer organic film is also improved. Accordingly, the adhesion promoter that has undergone the hydrolysis reaction and the dehydration reaction as described above is interposed between the substrate and the polymer organic film, thereby improving the adhesion between the substrate and the polymer organic film. It becomes like this.
- the content of the adhesion promoter in the aqueous solution is 20% by volume or more, and the heating temperature of the aqueous solution is 80 to 100 ° C.
- various amounts of the adhesion promoter are supplied to the substrate surface. This is a parameter condition obtained as a result of examining the parameters.
- water-containing adhesion promoter vapor means that the adhesion promoter vapor contains moisture regardless of the state.
- water-containing adhesion promoter vapor is obtained by heating an aqueous solution containing the adhesion promoter, in a narrow sense, it means a vapor formed by mixing the adhesion promoter vapor and water vapor. .
- the stock solution containing the adhesion promoter and water are prepared separately, and the stock solution and the water are used as the predetermined adhesion promoter.
- Each of them is heated and vaporized independently so as to be maintained at a mixing ratio or higher. Therefore, vapor and water vapor of the adhesion promoter are attached and condensed on the surface of the substrate. Accordingly, on the surface, the adhesion promoter and water react with each other to cause hydrolysis, and a functional group rich in reactivity is exposed on the surface of the adhesion promoter.
- the vapor is attached and aggregated on the surface of the substrate, and then heat treatment is performed.
- the adhesion promoter is hydrolyzed and dehydrated, and the functional groups exposed on the surface of the adhesion promoter are chemically bonded to the surface of the substrate. Accordingly, the adhesion between the adhesion promoter and the substrate is improved.
- the adhesion between the adhesion promoter and the polymer organic film is also improved. Therefore, the adhesion promoter that has undergone the hydrolysis reaction and the dehydration reaction as described above is interposed between the substrate and the polymer organic film, so that the adhesion force between the substrate and the polymer organic film is improved. become.
- the amount of vapor of the adhesion promoter and the amount of water vapor are prepared. And can be controlled independently. That is, since the amount of adhesion promoter and water supplied to the target substrate surface can be freely controlled, the degree of hydrolysis and the like described above can be freely controlled. Accordingly, the adhesion between the substrate and the polymer organic film can be freely controlled.
- the heating and dehydrating heater heats the surface of the substrate to 100 ° C. or higher. Thereby, the heat dehydration reaction can be easily caused.
- the adhesion promoter is a silane coupling agent.
- Silane coupling agents are easily available and can generate hydroxyl groups rich in reactivity by the hydrolysis described above, and the hydroxyl groups are strongly bonded to oxygen and the like on the substrate surface through a thermal dehydration reaction. Therefore, based on the mechanism described above, the adhesion between the substrate and the polymer organic film to be formed can be improved.
- the above-described film forming apparatus and film forming method can be included in the polymer organic film forming apparatus and film forming method.
- adhesion between a substrate, particularly a semiconductor substrate and a polymer organic film can be improved without generating a residue due to the adhesion promoter on the substrate.
- FIG. 1 is a block diagram schematically showing an example of the configuration of the surface treatment apparatus of the present invention. In the present embodiment, the first processing apparatus and the first processing method will be described.
- a holding container 12 is disposed below the processing container 11, and a vaporizing heater 13 is provided below the holding container 12 so as to seal the processing container 11 from below. It has been.
- an aqueous solution L containing an adhesion promoter such as a silane coupling agent is placed in the holding container 12.
- the substrate S is supported above the holding container 12 by a substrate holder (not shown).
- a heating and dehydrating heater (not shown) is provided in the processing container 11 in the vicinity of the substrate S.
- the heater 13 for vaporization can be a heater using a general-purpose system such as a resistance heating system.
- the heater for heat dehydration can also be constructed from a general purpose one.
- the content of the adhesion promoter in the aqueous solution L is 20% by volume or more. This is a parameter condition for supplying a sufficient amount of the adhesion promoter to the surface of the substrate S in the processing method described later. A sufficient amount of the adhesion promoter is not supplied, and the effect of the present invention, that is, the adhesion between the substrate S and the polymer organic film to be formed later cannot be improved.
- the upper limit of the content of the adhesion promoter in the aqueous solution L is the maximum amount that the adhesion promoter can be dissolved in water.
- a silane coupling agent is used as the adhesion promoter, it is about 30% at room temperature.
- the aqueous solution L held in the holding container 12 by the vaporizing heater 13 is heated to 80 to 100 ° C. Then, the aqueous solution L is vaporized and water vapor and adhesion promoter vapor are generated.
- the heating temperature of 80 to 100 ° C. is a parameter condition for supplying a sufficient amount of the adhesion promoter to the surface of the substrate S.
- a sufficient amount of the adhesion promoter is not supplied, and the effect of the present invention, that is, the adhesion between the substrate S and the polymer organic film to be formed later cannot be improved.
- the holding container 12 Since the holding container 12 is held in the processing container 11, the water vapor and the adhesion promoter vapor diffuse upward in the processing container 11, adhere to the surface of the substrate S and aggregate. At this time, the adhesion promoter is hydrolyzed in the presence of water on the surface of the substrate S, and a functional group rich in reactivity is formed on the surface. For example, when a silane coupling agent is used as the adhesion promoter, a hydroxyl group is formed.
- the surface of the substrate S is heated with the heater for heating and dehydrating to cause a dehydrating condensation reaction on the adhesion promoter. Then, the functional group exposed on the surface of the adhesion promoter reacts with the substrate S and becomes firmly bonded. Accordingly, the adhesion between the adhesion promoter and the substrate S is improved.
- the adhesion between the adhesion promoter and the polymer organic film is also improved. Accordingly, the adhesion promoter that has undergone the hydrolysis reaction and the dehydration reaction as described above is interposed between the substrate S and the polymer organic film, thereby improving the adhesion between the substrate S and the polymer organic film. It becomes like this.
- the heating dehydration reaction can also be performed in a separate batch. That is, in the processing container 11 as shown in FIG. 1, only the water vapor and the adhesion promoter vapor from the holding container 12 are adhered and aggregated to the surface of the substrate S, and the subsequent hydrolysis is performed. By taking out the substrate S from the processing container 11 and placing it on the heating and dehydrating heater 13 ′ as shown in FIG. 2, the heating and dehydrating reaction can be caused.
- the relationship between the concentration of the adhesion promoter in the adhesion promoter aqueous solution L in the holding container 12 and the adhesion force between the polymer organic film formed via the adhesion promoter was examined. The results are shown in FIG. A silane coupling agent was used as the adhesion promoter, and a Si substrate was used as the substrate. The polymer organic film formed on the Si substrate was a polyimide film (thickness 1 ⁇ m).
- FIG. 4 shows that when the concentration of the adhesion promoter in the adhesion promoter aqueous solution L exceeds 20% by volume, the adhesion between the Si substrate and the polyimide film is remarkably increased.
- the evaluation of the adhesion force is performed by fixing a tension jig on the back surface of the Si substrate and the front surface of the polyimide film via an adhesive, pulling the tension jig in the vertical direction, and the polyimide film from the Si substrate. It was defined by the tensile strength at the time of peeling.
- FIG. 5 is a block diagram schematically showing another example of the configuration of the surface treatment apparatus of the present invention.
- the second processing apparatus and the second processing method will be described.
- a first holding container 22 and a second holding container 23 are disposed below the processing container 21, and further below the first holding container 22 and the second holding container 23.
- the first vaporizing heater 24 and the second vaporizing heater 25 are provided so as to seal the processing vessel 21 from below.
- a stock solution L 1 of an adhesion promoter such as a silane coupling agent is put, and in the second holding container 23, water is put.
- a substrate S is supported above the first holding container 22 and the second holding container 23 by a substrate holder (not shown). Furthermore, a heater for dehydration (not shown) is provided in the processing container 21 in the vicinity of the substrate S.
- the first vaporization heater 24 and the second vaporization heater 25 can be heaters using a general-purpose system such as a resistance heating system.
- the heater for heat dehydration can also be constructed from a general purpose one.
- the first vaporization heater 24 and the second vaporization heater 25 cause the adhesion promoter stock solution L1 that has entered the first holding container 22 and the water L2 that has entered the second holding container 23, respectively. Is heated to vaporize the stock solution L1 and the water L2. At this time, the first vaporization heater 24 and the second vaporization heater 25 generate a sufficient amount of steam from the stock solution L1 and the water L2 so that the adhesion promoter has a predetermined mixing ratio or more. Set to a suitable temperature. For example, the first vaporizing heater 24 is heated to about 200 ° C. or higher, specifically 250 ° C. to 260 ° C. On the other hand, the first vaporizing heater 25 heats to 80 ° C. to 100 ° C.
- the adhesion promoter vapor vaporized from the stock solution L1 and the water vapor evaporated from the water L2 are upward in the processing container 21. And adhere to the surface of the substrate S and aggregate. At this time, the adhesion promoter is hydrolyzed in the presence of water on the surface of the substrate S, and a functional group rich in reactivity is formed on the surface as in the first embodiment. For example, when a silane coupling agent is used as the adhesion promoter, a hydroxyl group is formed.
- the surface of the substrate S is heated by the heating and dehydrating heater to cause a dehydration condensation reaction on the adhesion promoter after hydrolysis. Then, the functional group exposed on the surface of the adhesion promoter reacts with the substrate S and becomes firmly bonded. Accordingly, the adhesion between the adhesion promoter and the substrate S is improved.
- the adhesion between the adhesion promoter and the polymer organic film is also improved. Accordingly, the adhesion promoter that has undergone the hydrolysis reaction and the dehydration reaction as described above is interposed between the substrate S and the polymer organic film, thereby improving the adhesion between the substrate S and the polymer organic film. It becomes like this.
- the amount of vapor of the adhesion promoter (raw solution L1) and the amount of water vapor (from the water L2) And can be controlled independently. That is, since the amount of adhesion promoter and water supplied to the target substrate S surface can be freely controlled, the degree of hydrolysis and the like described above can be freely controlled. Therefore, the adhesion between the substrate S and the polymer organic film can be freely controlled.
- fever dehydration reaction can also be performed by another batch as shown in FIG.
- FIG. 6 is a block diagram schematically showing another example of the configuration of the surface treatment apparatus of the present invention.
- the present embodiment is the second processing apparatus and the second processing method, and corresponds to a modification of the second embodiment.
- the substrate S is held in a processing container 31 by a substrate holder (not shown), and separately from the processing container 31, a first holding container 32 and a second holding container 33.
- a first holding chamber 36 and a second holding chamber 37 are separately provided.
- the first vaporization heater 34 and the second vaporization vessel are respectively provided below the first holding container 32 and below the second holding container 33, respectively.
- a vaporizing heater 35 is provided.
- a stock solution L1 of an adhesion promoter such as a silane coupling agent is placed, and in the third holding container 33, water is placed.
- the processing vessel 31 is connected to the first holding chamber 36 and the second holding chamber 37 via pipes 38 and 39, respectively.
- the pipes 38 and 39 are connected in the middle, but the processing vessel 31 and the first holding chamber 36 are connected by the pipe 38 without necessarily being connected.
- the processing container 31 and the second holding chamber 37 may be connected by a pipe 39.
- a heating / dehydrating heater (not shown) is provided close to the substrate S in the processing container 31.
- the first vaporization heater 34 and the second vaporization heater 35 can be heaters using a general-purpose system such as a resistance heating system.
- the heater for heat dehydration can also be constructed from a general purpose one.
- the first vaporization heater 34 and the second vaporization heater 35 are used to cause an adhesion promoter stock solution L1 that has entered the first holding container 32 and water L2 that has entered the second holding container 33, respectively. Is heated to vaporize the stock solution L1 and the water L2. At this time, the first vaporization heater 34 and the second vaporization heater 35 generate a sufficient amount of steam from the stock solution L1 and the water L2 so that the adhesion promoter has a predetermined mixing ratio or more. Set to a suitable temperature. For example, the first vaporizing heater 34 is heated to about 200 ° C. or higher, specifically 250 ° C. to 260 ° C. On the other hand, the first vaporizing heater 35 heats to 80 ° C. to 100 ° C.
- a carrier gas can be flowed together with the adhesion promoter and water vapor to assist the introduction of the adhesion promoter vapor and the water vapor into the processing vessel 31.
- the surface of the substrate S is heated by the heating and dehydrating heater to cause a dehydration condensation reaction on the adhesion promoter after hydrolysis. Then, the functional group exposed on the surface of the adhesion promoter reacts with the substrate S and becomes firmly bonded. Accordingly, the adhesion between the adhesion promoter and the substrate S is improved.
- the adhesion between the adhesion promoter and the polymer organic film is also improved. Accordingly, the adhesion promoter that has undergone the hydrolysis reaction and the dehydration reaction as described above is interposed between the substrate S and the polymer organic film, thereby improving the adhesion between the substrate S and the polymer organic film. It becomes like this.
- the amount of vapor of the adhesion promoter (raw solution L1) and the amount of water vapor (from the water L2) And can be controlled independently. That is, since the amount of adhesion promoter and water supplied to the target substrate S surface can be freely controlled, the degree of hydrolysis and the like described above can be freely controlled. Therefore, the adhesion between the substrate S and the polymer organic film can be freely controlled.
- fever dehydration reaction can also be performed by another batch as shown in FIG.
- FIG. 7 is a configuration diagram schematically showing an example of the film forming apparatus of the present invention.
- a film forming apparatus 40 shown in FIG. 7 has a film forming container 41, and a plurality of substrates S are held inside the film forming container 41 by a substrate support container such as a boat (not shown).
- a substrate support container such as a boat (not shown).
- piping 42 for introducing the adhesion promoter vapor and water vapor obtained in the above embodiment and piping 43 for introducing the raw material monomer are alternately provided.
- an exhaust pipe 45 connected to an exhaust system (not shown) is provided on the right side of the film forming container 41.
- the pipe 43 is connected to the holding container 12 as shown in FIG. 1 and FIG. 5 or the part surrounded by the broken line as shown in FIG. Has been introduced in.
- the substrate S is disposed in the film forming container 41, the heating and dehydrating heaters in the surface treatment apparatuses 10, 20, and 30 shown in FIGS. Instead, it is provided in the film forming container 41.
- the substrate S is held at a predetermined temperature, the raw material monomer is introduced into the film formation container 41 from the pipe 42, and a thermal polymerization reaction is caused to form a polymer organic film on the surface of the substrate S.
- the adhesion promoter is interposed between the substrate S and the polymer organic film, so that the adhesion between the substrate S and the polymer organic film is improved.
- FIG. 8 is a configuration diagram schematically showing another example of the film forming apparatus of the present invention.
- a film forming apparatus 50 shown in FIG. 8 has a first film forming container 51 A and a second film forming container 51 B, and these film forming containers are connected to each other through a gate valve 57.
- a pipe 52 for introducing the adhesion promoter vapor and water vapor obtained in the above embodiment is provided on the lower surface of the first film formation container 51A, and a raw material is formed on the lower surface of the second film formation container 51B.
- a pipe 53 for introducing the monomer is provided.
- exhaust pipes 55A and 55B connected to an exhaust system (not shown) are provided to the right of each film forming container.
- a plurality of substrates S are held apart from each other by a substrate support container such as a boat (not shown).
- the piping 52 is connected to a holding container 12 as shown in FIGS. 1 and 5 or a portion surrounded by a broken line as shown in FIG. 6, and a vaporized adhesion promoter aqueous solution or the like is formed into a film. It is introduced into the container 51A. Also in this case, since the substrate S is disposed in the film forming container 51A, the heating and dehydrating heaters in the surface treatment apparatuses 10 and 20, and 30 shown in FIGS. Instead of 31, it is provided in the film forming container 41 ⁇ / b> A.
- the raw material monomer is introduced into the film forming container 51B from the pipe 53.
- the film forming apparatus 50 of the present embodiment performs pretreatment of the substrate S with the water-containing adhesion promoter vapor (water vapor and adhesion promoter vapor) in the first film formation container 51A, and performs the second film formation.
- the film forming process is performed by introducing the raw material monomer in the container 51B.
- the film forming apparatus 50 shown in FIG. 8 as described in the surface treatment apparatuses 10, 20, and 30 shown in FIG. 1, FIG. 5, and FIG.
- the accelerator vapor and the water vapor are generated, they are introduced into the first film forming container 51A through the pipe 52, and the hydrolysis reaction and the heat dehydration reaction are caused in the film forming container 51A (the surface of the substrate S).
- Squeeze pre-processing
- Excess adhesion promoter vapor or the like is exhausted from the film forming container 51A to the outside through the exhaust pipe 55A.
- the substrate S (the substrate support container) is moved into the second film forming container 51B
- the substrate S is held at a predetermined temperature
- the raw material monomer is introduced into the second film forming container 51B from the pipe 53, and heat is applied.
- a polymerization reaction is caused to form a polymer organic film on the surface of the substrate S.
- the adhesion promoter is interposed between the substrate S and the polymer organic film, so that the adhesion between the substrate S and the polymer organic film is improved.
- the gate valve 57 provided between the first film formation container 51A and the second film formation container 51B is closed between the pretreatment and the film formation process so that the atmosphere in each container does not interfere with each other. To. Further, the excess raw material monomer that does not contribute to the thermal polymerization reaction is exhausted to the outside from the film formation container 51B through the exhaust pipe 55B.
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Abstract
Description
本発明は、上述した問題に鑑み、基板上に密着促進剤に起因した残留物を発生させることなく、基板、特に半導体基板と高分子有機膜との密着性を向上させることを目的とする。
上記目的を達成すべく、本発明は、
20体積%以上の密着促進剤を含む水溶液の保持容器と、
前記保持容器内の前記水溶液を80~100℃の温度で加熱及び気化し、水含有密着促進剤蒸気を生成するための気化用ヒータと、
基板の表面に前記水含有密着促進剤蒸気が付着し凝縮した後、加熱脱水反応を生ぜしめて、前記基板の前記表面に前記密着促進剤を化学結合させる加熱脱水用ヒータと、
少なくとも前記保持容器を収納し、前記密着促進剤蒸気を保持するための処理容器と、
を具えることを特徴とする、基板の表面処理装置(第1の処理装置)に関する。
密着促進剤の原液を保持する第1の保持容器と、
水を保持する第2の保持容器と、
前記第1の保持容器内の前記密着促進剤の原液を加熱及び気化して、密着促進剤蒸気を生成するための第1の気化用ヒータと、
前記第2の保持容器内の前記水を加熱及び気化して、水蒸気を生成するための第2の気化用ヒータと、
基板の表面に前記密着促進剤が所定の混合比以上に保持された前記密着促進剤蒸気及び前記水蒸気が付着し加水分解した後、前記基板の前記表面に前記密着促進剤を化学結合させる加熱脱水用ヒータと、
少なくとも前記第1の保持容器及び前記第2の保持容器を収納し、前記密着促進剤蒸気及び前記水蒸気を保持するための処理容器と、
を具えることを特徴とする、基板の表面処理装置(第2の処理装置)に関する。
20体積%以上の密着促進剤を含む水溶液を保持容器内に保持する工程と、
前記水溶液を気化用ヒータで80~100℃の温度に加熱及び気化し、水含有密着促進剤蒸気を生成し、処理容器内に保持する工程と、
基板の表面に前記水含有密着促進剤蒸気を付着及び凝縮させた後、加熱脱水用ヒータで加熱脱水反応を生ぜしめて、前記基板の前記表面に前記密着促進剤を脱水縮合させる工程と、
を具えることを特徴とする、基板の表面処理方法(第1の処理方法)に関する。
密着促進剤の原液を第1の保持容器内に保持する工程と、
水を第2の保持容器内に保持する工程と、
前記第1の保持容器内の前記密着促進剤の原液を第1の気化用ヒータで加熱及び気化して、密着促進剤蒸気を生成し、処理容器内に保持する工程と、
前記第2の保持容器内の前記水を第2の気化用ヒータで加熱及び気化して、水蒸気を生成し、前記処理容器内に保持する工程と、
基板の表面に前記密着促進剤が所定の混合比以上に保持された前記密着促進剤蒸気及び前記水蒸気が付着し加水分解した後、加熱脱水用ヒータで脱水縮合させて、前記基板の前記表面に前記密着促進剤を化学結合させる工程と、
を具えることを特徴とする、基板の表面処理方法(第2の処理方法)に関する。
以上、本発明によれば、基板上に密着促進剤に起因した残留物を発生させることなく、基板、特に半導体基板と高分子有機膜との密着性を向上させることができる。
図1は、本発明の表面処理装置の構成の一例を概略的に示す構成図である。なお、本実施形態では、上記第1の処理装置及び上記第1の処理方法について説明する。
図5は、本発明の表面処理装置の構成の他の例を概略的に示す構成図である。なお、本実施形態では、上記第2の処理装置及び上記第2の処理方法について説明する。
図6は、本発明の表面処理装置の構成のその他の例を概略的に示す構成図である。なお、本実施形態は、上記第2の処理装置及び上記第2の処理方法であって、上記第2の実施形態の変形例に相当する。
本実施形態では、上述した実施形態における表面処理装置及び表面処理方法を用いた成膜装置及び成膜方法について説明する。
図8は、本発明の成膜装置の他の例を概略的に示す構成図である。図8に示す成膜装置50は第1の成膜容器51A及び第2の成膜容器51Bを有し、これらの成膜容器はゲートバルブ57を介して互いに連結されている。また、第1の成膜容器51Aの下面には、上記実施形態で得た密着促進剤蒸気及び水蒸気を導入するための配管52が設けられ、第2の成膜容器51Bの下面には、原料モノマーを導入するための配管53が設けられている。さらに、各成膜容器の右方には、図示しない排気系に接続された排気管55A及び55Bが設けられている。
Claims (10)
- 20体積%以上の密着促進剤を含む水溶液の保持容器と、
前記保持容器内の前記水溶液を80~100℃の温度で加熱及び気化し、水含有密着促進剤蒸気を生成するための気化用ヒータと、
基板の表面に前記水含有密着促進剤蒸気が付着し凝縮した後、加熱脱水反応を生ぜしめて、前記基板の前記表面に前記密着促進剤を化学結合させる加熱脱水用ヒータと、
少なくとも前記保持容器を収納し、前記密着促進剤蒸気を保持するための処理容器と、
を具えることを特徴とする、基板の表面処理装置。 - 密着促進剤の原液を保持する第1の保持容器と、
水を保持する第2の保持容器と、
前記第1の保持容器内の前記密着促進剤の原液を加熱及び気化して、密着促進剤蒸気を生成するための第1の気化用ヒータと、
前記第2の保持容器内の前記水を加熱及び気化して、水蒸気を生成するための第2の気化用ヒータと、
基板の表面に前記密着促進剤が所定の混合比以上に保持された前記密着促進剤蒸気及び前記水蒸気が付着し加水分解した後、前記基板の前記表面に前記密着促進剤を化学結合させる加熱脱水用ヒータと、
少なくとも前記第1の保持容器及び前記第2の保持容器と連続し、前記密着促進剤蒸気及び前記水蒸気を保持するための処理容器と、
を具えることを特徴とする、基板の表面処理装置。 - 前記加熱脱水用ヒータは、前記基板の前記表面を100℃以上に加熱することを特徴とする、請求項1又は2に記載の基板の表面処理装置。
- 前記密着促進剤は、シランカップリング剤であることを特徴とする、請求項1~3のいずれか一に記載の基板の表面処理装置。
- 請求項1~4のいずれか一に記載の基板の表面処理装置を具えることを特徴とする、有機膜の成膜装置。
- 20体積%以上の密着促進剤を含む水溶液を保持容器内に保持する工程と、
前記水溶液を気化用ヒータで80~100℃の温度に加熱及び気化し、水含有密着促進剤蒸気を生成し、処理容器内に保持する工程と、
基板の表面に前記水含有密着促進剤蒸気を付着及び凝縮させた後、加熱脱水用ヒータで加熱脱水反応を生ぜしめて、前記基板の前記表面に前記密着促進剤を脱水縮合させる工程と、
を具えることを特徴とする、基板の表面処理方法。 - 密着促進剤の原液を第1の保持容器内に保持する工程と、
水を第2の保持容器内に保持する工程と、
前記第1の保持容器内の前記密着促進剤の原液を第1の気化用ヒータで加熱及び気化して、密着促進剤蒸気を生成し、処理容器内に保持する工程と、
前記第2の保持容器内の前記水を第2の気化用ヒータで加熱及び気化して、水蒸気を生成し、前記処理容器内に保持する工程と、
基板の表面に前記密着促進剤が所定の混合比以上に保持された前記密着促進剤蒸気及び前記水蒸気が付着し加水分解した後、加熱脱水用ヒータで脱水縮合させて、前記基板の前記表面に前記密着促進剤を化学結合させる工程と、
を具えることを特徴とする、基板の表面処理方法。 - 前記加熱脱水用ヒータによって、前記基板の前記表面を100℃以上に加熱することを特徴とする、請求項6又は7に記載の基板の表面処理方法。
- 前記密着促進剤は、シランカップリング剤であることを特徴とする、請求項6~8のいずれか一に記載の基板の表面処理方法。
- 請求項6~9のいずれか一に記載の基板の表面処理方法を具えることを特徴とする、有機膜の成膜方法。
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JP6020239B2 (ja) * | 2012-04-27 | 2016-11-02 | 東京エレクトロン株式会社 | 成膜方法及び成膜装置 |
JP6322598B2 (ja) * | 2014-08-22 | 2018-05-09 | 東京エレクトロン株式会社 | 疎水化処理方法、疎水化処理装置及び疎水化処理用記録媒体 |
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