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
  • H01L21/02041—Cleaning
  • H01L21/02082—Cleaning product to be cleaned
  • H01L21/02087—Cleaning of wafer edges
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D9/00—Chemical paint or ink removers
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
  • C09D183/16—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers in which all the silicon atoms are connected by linkages other than oxygen atoms
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
  • C09D7/20—Diluents or solvents
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
  • C11D7/22—Organic compounds
  • C11D7/24—Hydrocarbons
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
  • C11D7/22—Organic compounds
  • C11D7/26—Organic compounds containing oxygen
• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D7/00—Compositions of detergents based essentially on non-surface-active compounds
  • C11D7/50—Solvents
• • 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
  • H01L21/02205—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 the layer being characterised by the precursor material for deposition
  • H01L21/02208—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 the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si
  • H01L21/02219—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 the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound comprising silicon and nitrogen
  • H01L21/02222—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 the layer being characterised by the precursor material for deposition the precursor containing a compound comprising Si the compound comprising silicon and nitrogen the compound being a silazane

Definitions

• the present invention relates to a polysilazane treatment solvent suitably used for treating a polysilazane coating film or polysilazane coating film formed on a substrate, and a polysilazane compound or polysilazane coating film using this solvent. It relates to the processing method.
• the present invention provides a polysilazane treatment solvent and a treatment method that can be suitably used for edge bead removal treatment in which a polysilazane coating film is formed on a substrate and then the edge portion of the coating film is treated.
• a siliceous film is used as an insulating film, a dielectric film, a protective film, a hydrophilic film, or the like.
• Methods for forming such a siliceous film on a substrate include physical vapor deposition methods such as sputtering (hereinafter referred to as PVD methods) and chemical vapor deposition methods (hereinafter referred to as CVD methods).
• PVD methods physical vapor deposition methods
• CVD methods chemical vapor deposition methods
• Various methods are used, such as a sol-gel method and a method of forming a polysiloxane or polysilazane coating film and converting the coating film into a siliceous film by baking or the like.
• the PVD method and the CVD method have problems that the apparatus is expensive and the control for forming a good-quality coating film is complicated.
• the Zonole-gel method has a problem that the required firing temperature is as high as 500 ° C or higher.
• the method using polysiloxane has problems such as generation of cracks due to a decrease in film thickness of the formed film.
• a method of applying a solution of a polysilazane compound hereinafter, various polysilazane compounds are sometimes collectively referred to as polysilazane for the sake of simplicity
• converting the coating film into a siliceous film is as follows. In recent years, it has attracted particular attention because it can easily form a siliceous film having excellent characteristics by low-temperature firing and the film quality of the formed siliceous film is also excellent.
• Such a siliceous film is widely used as an inter-layer insulating film, a planarizing film, a passivation film, an inter-element isolation insulator of a semiconductor element such as an LSI or a TFT liquid crystal display device.
• a siliceous film is widely used as an inter-layer insulating film, a planarizing film, a passivation film, an inter-element isolation insulator of a semiconductor element such as an LSI or a TFT liquid crystal display device.
• a polysilazane solution is spin-coated on a substrate having a step or no step where a semiconductor, wiring, electrode, etc.
• a processing solvent is usually applied or sprayed to the peripheral edge of the polysilazane coating film formed on the front side of the substrate.
• EBR process that removes the polysilazane coating film on the peripheral edge
• Back rinse is done
• the polysilazane film formed by coating by such a method may be required to be peeled off from the substrate in accordance with the necessity of subsequent processing, or may be applied to a spin coater or the like. It is also necessary to clean and remove the polysilazane adhering to the apparatus.
• the siliceous film formed from the polysilazane coating film is not only a semiconductor element but also a dielectric film such as a liquid crystal display device and a plasma display panel (PDP), an insulating film, or an insulating film. It is used in various fields as a wall film, etc., and as a protective coating for various articles such as car body surfaces such as automobiles, interiors and exteriors of houses, glass products, ceramics, and plastic products. As in the case of manufacturing, there may be a problem that the polysilazane film adhering to unnecessary portions must be removed.
• Patent Document 1 includes xylene, anisole, decalin, cyclohexane, cyclohexene, methylcyclohexane, ethylcyclohexane, limonene, hexane, octane, nonane, decane, C8-C11 alkane mixture, C8- C11 aromatic hydrocarbon mixture, aliphatic Z cycloaliphatic hydrocarbon mixture containing 5 wt% or more and 25 wt% or less of C8 or more aromatic hydrocarbon, and polysilazane containing dibutyl ether or a mixture thereof A processing solvent is disclosed.
• Such a processing solvent is also used for EBR processing, but at the edge-cut portion when EBR processing is performed, a film thickness rise called a hump is formed at the boundary between the film and the portion from which the film has been removed. Since this hump causes cracks and peeling of the film when the film is baked, a processing solvent capable of obtaining a film having a more excellent shape of the edge cut after the EBR process has been desired.
• Patent Document 1 Japanese Patent Laid-Open No. 2003-197611
• Patent Document 2 Japanese Patent Application Laid-Open No. 11-105185
• the present invention relates to a polysilazane treatment solvent that does not have the above-described problems during EBR treatment during production of a polysilazane coating film, or rinsing or peeling of a polysilazane coating film, and a polysilazane compound or polysilazane coating film using the same. Eye to provide a processing method It is intended.
• the shape of the edge cut portion is good, and the polysilazane treatment solvent and the polysilazane are treated using this solvent. It aims to provide a method.
• the present invention is a polysilazane-treated solvent that is excellent in solubility of polysilazane and does not affect the properties of the underlying semiconductor or substrate and the properties of the remaining polysilazane coating film. And a method for treating polysilazane using this solvent.
• the first polysilazane treatment solvent according to the present invention comprises a solvent selected from the group consisting of tetralin, p-menthane, p-cymene, ⁇ -pinene, 1,8-cineol, and mixtures thereof. It is characterized by.
• the second polysilazane treatment solvent according to the present invention is a solvent selected from the group consisting of tetralin, ⁇ -menthane, ⁇ -cymene, hibinene, 1,8-cineole, and mixtures thereof.
• the first polysilazane compound treatment method according to the present invention is characterized in that any of the above polysilazane treatment solvents is brought into contact with a polysilazane compound.
• the edge portion of the polysilazane coating film formed on the substrate or the polysilazane coating film is not formed.
• the polysilazane coating film is treated by spraying any one of the above-mentioned polysilazane treatment solutions onto the back surface of the substrate.
• a processing solvent in which the shape of the edge cut portion is good when used in EBR processing.
• This treatment solvent is excellent in solubility in polysilazane, has excellent stability when mixed with polysilazane, and also has the characteristics of not affecting the properties of the substrate substrate, polysilazane compound or coating film. It can also be suitably used for back rinse when the coating solution is applied to the substrate. Furthermore, the treatment according to the present invention. Physical solvents are also highly safe for the human body.
• FIG. 1 is a cross-sectional view of a substrate surface after being treated with a treatment solvent.
• the polysilazane treatment solvent in the present invention comprises a solvent selected from the group 1 consisting of tetralin, p-menthane, p-cymene, hy-pinene, 1,8-cineole, and mixtures thereof.
• a solvent selected from this group is mixed and used, the mixing ratio is not particularly limited.
• another polysilazane treatment solvent in the present invention is a solvent selected from the group consisting of tetralin, p-menthane, p-cymene, ⁇ -vinene, 1,8-cineole, and mixtures thereof.
• solvents included in Group 2 are hexane, octane, nonane, decane, decalin, undecane, dodecane, tridecane, tetradecane, isononane, isodecane, isondecane, isododecane, isotridecane, isodecane
• examples include tetradecane, cyclononane, cyclodecane, cycloundecane, cyclododecane, cyclotridecane, and cyclotetradecane.
• aliphatic hydrocarbons and alicyclic hydrocarbons used as solvents included in Group 2.
• the compounding ratio in each of Group 1 or Group 2 is not particularly limited, but it is preferable that the solvent of Group 1 is 10% by weight or more based on the weight of the whole processing solvent. preferable. Generally, the higher the compounding ratio of Group 1 solvent, the higher the solubility and edge cut. The partial shape tends to be good, so it is preferable, but the flash point can be adjusted by adding the solvent of group 2 so that it can be adjusted from the viewpoint of safety.In general, the solvent of group 1 is expensive because it is expensive. From this viewpoint, it is also preferable that a solvent of Group 2 is blended.
• the following are particularly preferable because the shape of the edge cut portion which is particularly important in the EBR processing of the semiconductor substrate tends to be good.
• a processing solvent selected from the group consisting of tetralin, p-menthane, p-cymene, and mixtures thereof.
• the number of fine particles of 0.5 microns or more contained in 1 ml of the treatment solvent in the present invention is preferably 50 or less, more preferably 10 or less.
• the content of fine particles of 0.5 microns or more in lml of the treatment solvent exceeds 50, the fine particles in the treatment solvent are removed by appropriate means such as filtration and distillation, and contained in 1ml of the solvent.
• the number of fine particles of 5 microns or more is 50 or less, it is possible to reduce the number of fine particles.
• the number of fine particles of 0.5 microns or more contained in lml of the processing solvent exceeds 50, it is often observed that fine particles remain in the treated polysilazane film.
• the treatment solvent of the present invention can be mixed with other solvents within a range that does not impair the effects of the present invention.
• aromatic hydrocarbons have the effect of increasing the solubility of polysilazane and can be added to increase the solubility of the processing solvent.
• aromatic hydrocarbon solvents such as C8-C11 aromatic hydrocarbon mixtures (for example, Solvesso 100, Solvesso 150 (made by Shell Oil Corporation, USA).
• an aliphatic Z alicyclic hydrocarbon mixture containing 5 to 25% by weight of C8 or more aromatic hydrocarbons eg Vegasol AN45 (trade name, manufactured by ExxonMobil, USA)
• the amount is preferably 50% by weight or less, more preferably 20% by weight or less, of the treatment solvent according to the invention.
• the processing solvent according to the present invention may be diluted using mineral spirit as a diluent solvent within a range in which the object of the present invention can be achieved.
• the number of fine particles of 0.5 microns or more contained in lml of the mineral spirit used at this time is preferably 50 or less.
• methylcyclohexane, ethylcyclohexane, and the like have a low odor, when odorlessness is required, a solvent having such a low odor may be selected.
• Pegasol AN45 (trade name) is a hydrorefined fraction of the spilled oil obtained by atmospheric distillation of crude oil, and is a petroleum hydrocarbon mainly in the C8 to C11 range with an aniline point. It is f night body at 43 ° C.
• the treatment solvent of the present invention preferably has a water content of 80 ppm or less, preferably 10OOppm or less. If the water content is less than lOOppm, gelation due to decomposition of polysilazane in contact with the solvent tends to be slowed.For example, it takes time to remove the polysilazane adhering to the spin coater's waste liquid line, spin coater, etc. This is preferable because problems such as force and burrs can be suppressed.
• the treatment solvent according to the present invention can be generally applied to any polysilazane, but depending on the type of polysilazane, that is, what structure or composition of the polysilazane to be treated is. As a result, the optimum processing solvent varies. This is because the solubility of polysilazane is the same as that used as the processing solvent, even though the polysilazane is an organic polysilazane that is an inorganic polysilazane, a single polymer or copolymer force, and a copolymer.
• the optimum solvent may be selected from the above-mentioned solvents according to the present invention depending on the structure or composition of the polysilazane to be treated.
• the polysilazane to which the treatment solvent of the present invention is applied may be either inorganic or organic.
• examples of the inorganic polysilazane include a general formula:
• each weight of 6-5-7-5 0/0 which is perhydropolysilazane, and polystyrene-reduced average molecular weight of 3, 000 to 20, and a perhydropolysilazane in the range of 000.
• perhydropolysilazanes can be produced by any method, and basically include a chain portion and a cyclic portion in the molecule. [Chemical 2]
• polysilazanes include, for example, a general formula:
• R 2 and R 3 are each independently a hydrogen atom, an alkyl group, an alkenyl group, a cycloalkyl group, an aryl group, or a group other than these groups, in which the group directly connected to the carbon such as a fluoroalkyl group is a carbon, an alkyl Represents a silyl group, an alkylamino group or an alkoxy group.
• At least one of R 2 and R 3 is a hydrogen atom.
• polysilazanes to which the polysilazane treatment solvent according to the present invention can be applied include polyorgano (hydro) silazane having a hydrogen atom in R 1 and R 2 and an organic group in R 3 in the general formula (II), (R 2 SiHNH) — as a repeating unit, mainly has a cyclic structure with a degree of polymerization of 3 to 5.
• R SiHNH [(R SiH) N] (0 ⁇ 4 ⁇ X ⁇ 1)
• organic polysilazanes other than the above general formula (II) include, for example, the general formula:
• Examples thereof include polysilazane having a structure.
• repeating units are [(SiH 4) (NH)] and [(SiH 4)] (in these formulas, n, m,
• r is 1, 2 or 3, respectively) modified polysilazane, metal obtained by adding a terminal N atom with alcohol such as methanol or hexamethyldisilazane to perhydropolysilazane.
• alcohol such as methanol or hexamethyldisilazane
• perhydropolysilazane examples thereof include metal-containing polysilazane containing aluminum.
• polysilazane inorganic silazane high polymer, modified polysilazane, copolymerization
• Low-temperature ceramicized polysilazane with addition or addition of a catalytic compound to promote ceramicization to polysilazane polysilazane with alkoxide addition
• polysilazane with addition of glycidol polysilazane with addition of acetylethylacetonate complex
• compositions obtained by adding amines or / and acids to various polysilazanes or modified products as described above.
• the form of polysilazane to which the solvent of the present invention is applied is usually a film form, but is not limited to a film form.
• the method of coating the polysilazane on the substrate is any of the conventionally known methods such as spin coating, spray coating, flow coating, roller coating, dip coating, cloth wiping, and sponge wiping. It ’s okay, and it ’s not limited.
• the shape of the substrate may be plate-like or film-like, and the surface state may be flat, uneven, or curved.
• the material of the substrate may be any material such as semiconductor, glass, metal, metal oxide, and plastic.
• the method of bringing the solvent of the present invention into contact with polysilazane is not limited in any way, and spraying or spraying of the solvent from the nozzle onto the polysilazane on the substrate, in the solvent of the substrate coated with polysilazane. Any method may be used such as immersion in water, washing of polysilazane with a solvent, and pouring.
• a semiconductor substrate silicon wafer
• a polysilazane solution and an interlayer insulating film, a planarizing film, a passivation film, an inter-element isolation film, or the like is formed on the semiconductor substrate
• a spin coater if necessary, for example, on a wafer that rotates at a rotational speed of 500 to 4000 rpm.
• Time to spray treatment solvent 0.01 to 60 seconds
• back-rinsing can be simultaneously performed by spraying a polysilazane treatment solvent onto the back surface of the substrate.
• EBR treatment and back rinsing can be performed independently. It is preferable because the steps can be omitted by performing them simultaneously.
• the gelling days are preferably 2 days or more, more preferably 3 days or more.
• a 100 g glass bottle was mixed with 5 g of a 20% by weight di-n-butyl ether solution of each polysilazane compound and 50 g of a processing solvent, mixed, sealed, and after 1 hour, the gas phase portion was sampled and measured with a gas chromatograph.
• the film thickness 4 of this raised part was measured with a reflection spectral film thickness meter FE-3000 manufactured by Otsuka Electronics Co., Ltd. to evaluate the raised film thickness of the edge cut part.
• the rise of the edge cut portion is preferably less than lxm practically.
• the back surface was evaluated by observing with an optical microscope and checking for residuals.
• Example 1 4 0.001 0.05 0 Good
• Example 2 3 0.003 0.1 0.1 Good
• Example 3 3 0.003 0.4 0.3 Good
• Example 4 5 0.003 0.05 2 Good
• Example 5 3 0.003 0.1 0 Good
• Example 6 3 0.003 0.1 0.1 Good
• Example 7 4 0.001 0.05 0.5 Good
• Example 8 2 0.01 0.1 0.5 Good
• Example 9 2 0.005 0.05 0.4 Good
• Example 10 2 0.002 0.05 0.4 Good
• Example 1 2 0.002 0.06 0.4 Good
• Example 12 2 0.002 0.1 0.4 Good
• Example 13 3 0.002 0.1 0 Good
• Example 14 3 0.004 0.04 0.3 Good
• Example 15 3 0.002 0.03 0.05 Good
• Example 16 3 0.002 0.02 0 Good
• Example 17 3 0.002 0.02 0 Good
• Example 18 4 0.003 0.02 0.6 Good
• Example 19 2 0.01 0.1 0.6 Good
• Example 20 2 0.003 0.05 0.6
• Example 1 7 0.001 0.05 0 Good
• Example 2 7 0.003 0.06 0.1 Good
• Example 3 7 0.02 0.1 0.2 Good
• Example 4 5 0.002 0.03 1.5 Good
• Example 5 6 0.002 0.05 0 Good
• Example 6 6 0.002 0.08 0.2 Good
• Example 7 6 0.001 0.04 0.4 Good
• Example 8 6 0.01 0.1 0.5 Good
• Example 9 7 0.002 0.06 0.3 Good
• Example 10 7 0.002 0.05 0.4 Good
• Example 1 7 0.002 0.04 0.4 Good
• Example 12 7 0.002 0.05 0.3 Good
• Example 13 7 0.002 0.05 0.1 Good
• Example 14 7 0.003 0.04 0.3 Good
• Example 15 7 0.001 0.03 0.1 Good
• Example 16 7 0.001 0.01 0 Good
• Example 17 7 0.003 0.01 0 Good
• Example 18 7 0.003 0.02 0.6 Good
• Example 19 7 0.005 0.1 0.5 Good
• Example 20 7 0.002 0.01 0.6
• Example 1 3 0.001 0.05 0 Good
• Example 2 2 0.003 0.1 0 Good
• Example 3 2 0.003 0.4 0 Good
• Example 4 3 0.003 0.05 0.15 Good
• Example 5 2 0.003 0.1 0 Good
• Example 6 2 0.003 0.1 0 Good
• Example 7 3 0.001 0.05 0.1 Good
• Example 8 2 0.01 0.1 0.1 Good
• Example 9 1 0.005 0.05 0.1 Good
• Example 10 1 0.002 0.05 0.1 Good
• Example 1 1 1 0.002 0.06
• Example 12 1 0.002 0.1 0.1 Good
• Example 13 1 0.002 0.1 0 Good
• Example 14 1 0.004 0.04 0 Good
• Example 15 1 0.002 0.03
• Example 16 1 0.002 0.02
• Example 17 1 0.002 0.02 0 Good
• Example 18 3 0.003 0.02 0.2 Good
• Example 19 2 0.01 0.1 0.2 Good
• Example 20 1 0.003 0.05
• the treatment solvent according to the present invention has a gelation days, a gas generation amount, an edge cut. Both the shape of the portion has been improved, I to be more excellent processing solvent Chikararu c

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• 2005
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