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WO2020116270A1 - Composition pour diffusion d'impuretés du type p et son procédé de production, procédé de fabrication d'élément à semi-conducteur utilisant ladite composition pour diffusion, et batterie solaire - Google Patents

Composition pour diffusion d'impuretés du type p et son procédé de production, procédé de fabrication d'élément à semi-conducteur utilisant ladite composition pour diffusion, et batterie solaire Download PDF

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WO2020116270A1
WO2020116270A1 PCT/JP2019/046319 JP2019046319W WO2020116270A1 WO 2020116270 A1 WO2020116270 A1 WO 2020116270A1 JP 2019046319 W JP2019046319 W JP 2019046319W WO 2020116270 A1 WO2020116270 A1 WO 2020116270A1
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Prior art keywords
type impurity
impurity diffusion
diffusion composition
semiconductor substrate
film
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Japanese (ja)
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北田剛
橘邦彦
秋本旭
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Toray Industries Inc
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Toray Industries Inc
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Priority to CN201980077286.4A priority Critical patent/CN113169247A/zh
Priority to JP2019565963A priority patent/JP7463725B2/ja
Publication of WO2020116270A1 publication Critical patent/WO2020116270A1/fr
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    • 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
    • H01L21/22—Diffusion of impurity materials, e.g. doping materials, electrode materials, into or out of a semiconductor body, or between semiconductor regions; Interactions between two or more impurities; Redistribution of impurities
    • H01L21/225—Diffusion of impurity materials, e.g. doping materials, electrode materials, into or out of a semiconductor body, or between semiconductor regions; Interactions between two or more impurities; Redistribution of impurities using diffusion into or out of a solid from or into a solid phase, e.g. a doped oxide layer
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F10/00—Individual photovoltaic cells, e.g. solar cells
    • H10F10/10—Individual photovoltaic cells, e.g. solar cells having potential barriers
    • H10F10/17—Photovoltaic cells having only PIN junction potential barriers
    • H10F10/174—Photovoltaic cells having only PIN junction potential barriers comprising monocrystalline or polycrystalline materials
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10F—INORGANIC SEMICONDUCTOR DEVICES SENSITIVE TO INFRARED RADIATION, LIGHT, ELECTROMAGNETIC RADIATION OF SHORTER WAVELENGTH OR CORPUSCULAR RADIATION
    • H10F71/00—Manufacture or treatment of devices covered by this subclass
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E10/00—Energy generation through renewable energy sources
    • Y02E10/50—Photovoltaic [PV] energy
    • Y02E10/547—Monocrystalline silicon PV cells
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the present invention relates to a composition for diffusing p-type impurities in a semiconductor substrate, a method for producing the composition, a method for producing a semiconductor device using the composition, and a solar cell.
  • the main method of forming a p-type or n-type impurity diffusion layer in a semiconductor substrate is to use a gas such as BBr 3 for p-type or POCl 3 for n-type substrate.
  • a gas such as BBr 3 for p-type or POCl 3 for n-type substrate.
  • the method of heating while contacting with is adopted.
  • thermal diffusion a method of forming an impurity diffusion layer by applying a composition containing a p-type or n-type impurity component onto a substrate and diffusing it by heat.
  • the diffusion of impurities into the substrate by heat from the composition containing the impurity component applied on the substrate may be referred to as thermal diffusion.
  • An impurity diffusion composition for forming a p-type impurity diffusion layer (hereinafter referred to as a p-type impurity diffusion composition) is prepared by mixing a compound containing a Group 13 element such as boron with a resin such as polyvinyl alcohol to form a complex. It is obtained by dissolving or dispersing the above in a solvent.
  • a solvent is preferably an organic solvent having a low surface tension. Since a resin such as polyvinyl alcohol for forming a complex by compounding a compound containing is often a water-soluble resin, the solvent of the actual composition is often a mixture of water and an organic solvent (for example, See Patent Documents 1 to 5).
  • the solvent is a mixture of water and an organic solvent
  • the complex of the compound containing the Group 13 element and polyvinyl alcohol is destabilized, the film thickness of the obtained coating film is reduced, and the impurities diffuse.
  • the in-plane uniformity of the sheet resistance value (impurity diffusion concentration) of the formed substrate is lowered, and the viscosity changes with time during storage of the p-type impurity diffusion composition.
  • the present invention has been made based on the above-mentioned circumstances, and uniformly diffuses impurities into a semiconductor substrate, improves the film thickness uniformity of a coating film, and improves the storage stability of a composition. It is an object of the present invention to provide a p-type impurity diffusion composition that enables the above.
  • the p-type impurity diffusion composition of the present invention has the following constitution. That is, (A) at least one resin selected from polyvinyl alcohol and polyethylene oxide, A p-type impurity diffusion composition comprising (b) a solvent, and (c) a compound containing a Group 13 element, wherein the p-type impurity diffusion composition has a pH of 4 to 6.5, and (b) the solvent. Contains (b-1) an organic solvent having a boiling point of 110° C. or higher and 210° C. or lower and (b-2) water, and the amount of (b-2) water is 10 to 50% by mass in the solvent (b). It is a p-type impurity diffusion composition characterized by the above.
  • a p-type impurity diffusion composition having excellent uniformity of impurity diffusion into a semiconductor substrate and film thickness of a coating film, and high storage stability.
  • FIG. 6 is a process cross-sectional view showing an example of a method for forming an impurity diffusion layer using the p-type impurity diffusion composition of the present invention.
  • FIG. 6 is a process cross-sectional view showing an example of a method for forming an impurity diffusion layer using the p-type impurity diffusion composition of the present invention. It is process sectional drawing which shows an example of the manufacturing method of the back junction solar cell using the p-type impurity diffusion composition of this invention.
  • FIG. 6 is a process cross-sectional view showing another example of a method for forming an impurity diffusion layer using the p-type impurity diffusion composition of the present invention.
  • FIG. 6 is a process cross-sectional view showing another example of a method for forming an impurity diffusion layer using the p-type impurity diffusion composition of the present invention.
  • FIG. 6 is a process cross-sectional view showing another example of a method for forming an impurity diffusion layer using the p-type impurity diffusion composition of the present invention.
  • the p-type impurity diffusion composition of the present invention is (A) at least one resin selected from polyvinyl alcohol and polyethylene oxide, A p-type impurity diffusion composition comprising (b) a solvent and (c) a compound containing a Group 13 element, wherein the composition has a pH of 4 to 6.5, and (b) the solvent is (b- 1) An organic solvent having a boiling point of 110° C. or higher and 210° C. or lower and (b-2) water, wherein the amount of water (b-2) is 10 to 50% by mass in the solvent (b). P-type impurity diffusion composition.
  • the p-type impurity diffusion composition of the present invention contains (a) at least one resin selected from polyvinyl alcohol and polyethylene oxide.
  • the resin (a) is a component for forming a complex with the compound (c) containing a Group 13 element and forming a uniform coating film during coating.
  • Polyvinyl alcohol is preferable from the viewpoint of the ability to form a complex with a compound containing a Group 13 element and the stability of the formed complex.
  • the average degree of polymerization of polyvinyl alcohol is preferably 150 to 1000 in terms of solubility and complex stability.
  • the saponification degree of polyvinyl alcohol is preferably 70 to 95 mol% in view of solubility and complex stability.
  • both the average degree of polymerization and the degree of saponification are values measured according to JIS K 6726 (1994).
  • the saponification degree is a value measured by the back titration method among those described in JIS.
  • the resin (a) contained in the p-type impurity diffusion composition is 80% by mass or more, preferably 90% by mass or more, and most preferably 95% by mass based on all the resins contained in the composition. It is preferably at least mass %.
  • the amount of the resin (a) depends on the composition in terms of (c) good thermal diffusion of the compound containing a Group 13 element into the semiconductor substrate and suppression of organic residues on the substrate after removal of the composition.
  • the content is preferably 0.1 to 20% by mass, more preferably 1 to 10% by mass, based on 100% by mass.
  • the p-type impurity diffusion composition of the present invention contains (b-1) an organic solvent having a boiling point of 110° C. or higher and 210° C. or lower. (B-1) When the boiling point of the organic solvent is within this range, after the p-type impurity diffusion composition is applied to the semiconductor substrate, (c) the compound including the Group 13 element and (a) the resin-based complex are dissolved. (B) water contained in the (b) solvent and (b-1) organic solvent volatilize in a well-balanced manner to obtain a coating film excellent in film thickness uniformity and impurity diffusion concentration uniformity. You can
  • the range of the boiling point of the organic solvent (b-1) is preferably 120° C. or higher and 185° C. or lower, more preferably 165° C. or higher and 180° C. or lower.
  • organic solvent (b-1) examples include dimethylformamide (boiling point 153° C., the same below), diethylene glycol monomethyl ether (193° C.), 1-butanol (118° C.), cyclohexanol (161° C.), ethylene glycol mono Ethyl ether acetate (156.4°C), ethylene glycol monomethyl ether acetate (145°C), methyl lactate (145°C), ethyl lactate (155°C), diacetone alcohol (169°C), 3-methoxy-3-methyl- 1-butanol (174°C), dipropylene glycol monomethyl ether (188°C), ⁇ -butyrolactone (204°C), ethyl acetoacetate (181°C), N-methyl-2-pyrrolidone (204°C), propylene glycol t- Butyl ether (151°C), propylene glycol n-butyl ether (170°C), acetylacetone (140, di
  • (B-1) Organic solvent in that the compatibility between the compound containing the Group 13 element (c) and the complex composed of the resin (a) is further improved, and the film thickness uniformity of the coating film is further improved.
  • the p-type impurity diffusion composition is characterized in that the complex formed from the compound containing the group 13 element (c) and the resin (a) becomes more stable and the storage stability of the p-type impurity diffusion composition is better.
  • the amount of the (b-1) organic solvent contained therein is preferably 50 to 90 mass% in the (b) solvent. It is more preferably 55 to 85 mass% in the solvent (b), and even more preferably 65 to 80 mass% in the solvent (b).
  • the p-type impurity diffusion composition of the present invention contains (b-2) water.
  • the amount of water (b-2) is 10 to 50 mass% in the solvent (b). Within this range, the complex formed from the compound containing the group 13 element (c) and the resin (a) is stable, and the p-type impurity diffusion composition has excellent storage stability.
  • the amount of water (b-2) is preferably 15 to 45% by mass in the solvent (b), and more preferably 20 to 35% by mass in the solvent (b).
  • the boiling point of the organic solvent (b-1) is 120° C. or higher and 185° C. or lower, and the amount of water (b-2) is 15 to 45 in the solvent (b).
  • the boiling point of the organic solvent (b-1) is 165° C. or higher and 180° C. or lower, and the amount of water (b-2) is 15 to 45% by weight in the solvent (b).
  • the boiling point of (b-1) the organic solvent is 165° C. or higher and 180° C. or lower, and (b-2) the amount of water is 20 to 35% by mass in the solvent (b). It is more preferable that there is.
  • the p-type impurity diffusion composition of the present invention includes (c) a compound containing a Group 13 element.
  • Examples of the Group 13 element include boron, aluminum, gallium, indium, thallium, and nihonium, and boron is preferably used from the viewpoint of diffusibility into a semiconductor substrate.
  • the compound containing boron include boric acid, boric acid such as diboron trioxide, borate salts such as ammonium borate, boron trifluoride, boron trichloride, boron tribromide, and triiodide.
  • examples thereof include halides such as boron, boronic acids such as methylboronic acid and phenylboronic acid, and borate esters such as trimethyl borate, triethyl borate, tripropyl borate, tributyl borate, trioctyl borate, and triphenyl borate. be able to.
  • boric acids, boronic acids, and boric acid esters are preferable from the viewpoint of easy handling.
  • the amount of the (c) Group 13 element compound contained in the p-type impurity diffusion composition can be arbitrarily determined according to the resistance value required for the semiconductor element, but is 0.05 or less with respect to the p-type impurity diffusion composition. It is preferably contained in an amount of up to 1% by mass. It is more preferably 0.1 to 0.5% by mass.
  • the mass ratio of (c) compound containing Group 13 element/(a) resin is more preferably 0.25 to 0.45.
  • the p-type impurity diffusion composition of the present invention preferably contains (d) a surfactant.
  • a surfactant By including the surfactant, the dispersibility of the compound containing the group 13 element (c) is increased, and the complex formation between the compound containing the group 13 element (c) and the resin (a) is improved. This can reduce organic residues on the substrate when the p-type impurity diffusion composition is removed after thermally diffusing the compound containing the group 13 element (c) into the semiconductor substrate.
  • a fluorine-based surfactant a silicone-based surfactant, an acrylic surfactant, etc. are preferably used.
  • fluorine-based surfactant examples include 1,1,2,2-tetrafluorooctyl (1,1,2,2-tetrafluoropropyl) ether and 1,1,2,2-tetrafluorooctyl.
  • fluorosurfactants include Megafac F142D, F172, F173, F183, F444, F475 and F477 (all manufactured by Dainippon Ink and Chemicals, Inc.) and Ftop.
  • F301, 303, 352 all manufactured by Shin-Akita Kasei Co., Ltd.
  • Florard FC-430, FC-431 all manufactured by Sumitomo 3M Limited
  • Asahi Guard AG710 Surflon S-382, and the same.
  • SC-101, SC-102, SC-103, SC-104, SC-105, SC-106 (above Asahi Glass Co., Ltd.), BM-1000, BM-1100 (above, Yusho) Fluorine-based surfactants such as NBX-15, FTX-218, DFX-218 (manufactured by Neos) and the like.
  • silicone-based surfactants include SH28PA, SH7PA, SH21PA, SH30PA, ST94PA (all manufactured by Toray Dow Corning Co., Ltd.), BYK067A, BYK310, BYK322, BYK331, BYK333, BYK355 (more, Big Chemie Japan. (Manufactured by Co., Ltd.) and the like.
  • Acrylic surfactants include Polyflow 77 and Polyflow 75 (all manufactured by Kyoeisha Chemical Co., Ltd.).
  • a silicone-based surfactant and/or an acrylic-based surfactant is used.
  • a surfactant is more preferably used.
  • (d) surfactant/( c) The mass ratio of the Group 13 element compound is preferably 0.03 to 0.1. This ratio is more preferably 0.03 to 0.045.
  • the p-type impurity diffusion composition of the present invention has a pH of 4 to 6.5. In this range, the complex of the resin (a) and the compound (c) containing the Group 13 element is stabilized. Further, even when the composition is stored for a certain period of time and then used for diffusion, the uniformity of the impurity diffusion concentration in the substrate surface can be kept good.
  • a more preferable range of pH is 4.5 to 5.5.
  • the method for adjusting the pH include, but are not limited to, a method of adding an acid and a base to the composition and a method of adjusting when impurities are reduced by the ion exchange resin as described later.
  • inorganic acids such as hydrochloric acid, sulfuric acid and nitric acid and organic acids such as acetic acid and oxalic acid are preferable, and sulfuric acid, nitric acid, acetic acid and oxalic acid containing no metal element or halogen are more preferable.
  • an organic amine containing no metal element or halogen is preferable.
  • a method of combining addition of an organic amine and addition of sulfuric acid, nitric acid, acetic acid or oxalic acid, or a method of combining addition of an organic amine and adjustment with an ion exchange resin is preferable.
  • Aromatic amines and aliphatic amines can be used as organic amines, but aliphatic amines, which have high basicity and are effective when added in smaller amounts, are preferred. From the viewpoint of suppressing side reactions with other components of the composition, a tertiary amine is more preferable.
  • aliphatic tertiary amine examples include, but are not limited to, trimethylamine, triethylamine, triisopropylamine, triisopropanolamine, triethanolamine, pyridine, piperazine, piperidine, pyrrolidine, ethylpiperidine, piperidineethanol and the like. .. Aliphatic cyclic tertiary amines such as piperazine, piperidine, pyrrolidine, ethyl piperidine, and piperidine ethanol are preferably used.
  • the content of the organic amine is preferably 0.01 to 2 mass% of the entire composition. It is more preferably 0.02 to 0.5% by mass of the entire composition, and even more preferably 0.03 to 0.1% by mass of the entire composition.
  • the pH in the present invention is a value measured using a pH meter (LAQUA F-71, manufactured by Horiba Ltd.).
  • the pH is calibrated using the following five types of standard solutions (pH 2, 4, 7, 9, 12) defined in JIS Z 8802:2011 “pH measuring method”.
  • the amount of sodium (Na) in the p-type impurity diffusion composition of the present invention is preferably 0.05 ppm or less.
  • a method for reducing Na a method in which each constituent of the composition is highly purified by recrystallization, distillation, column fractionation, ion exchange or the like is used, but a method using an ion exchange resin is preferable, and
  • the method for producing the p-type impurity diffusion composition preferably includes a step of performing an ion exchange treatment with an ion exchange resin.
  • the step of subjecting the entire composition containing the components (a) to (c) or at least one of the components (a) to (c) to the ion exchange treatment with an ion exchange resin Is raised. Since Na may be mixed in during the manufacturing process, it is most preferable to perform the ion exchange treatment at the end in the state of the whole composition containing the components (a) to (c).
  • a p-type impurity diffusion composition is passed through a column filled with a cation exchange resin.
  • the cation exchange resin is added to a liquid of the p-type impurity diffusion composition and stirred,
  • the ion exchange resin may be removed after the ion exchange, but the ion exchange resin is not limited thereto.
  • the pH of the p-type impurity diffusion composition after ion exchange will be less than 7, so it is possible to reduce impurities and adjust the pH to the target.
  • a method of performing ion exchange treatment by combining a cation exchange resin and an anion exchange resin is preferable.
  • a combination method a cation exchange resin and an anion exchange resin are appropriately mixed and packed in a column, and a p-type impurity diffusion composition is passed through, or a column packed with a cation exchange resin and an anion exchange resin are mixed. There is a method of continuously passing through a packed column, but not limited to these.
  • the viscosity of the p-type impurity diffusion composition of the present invention is not limited, and can be appropriately changed according to the coating method and the film thickness to be obtained.
  • the viscosity of the p-type impurity diffusion composition is preferably 1 to 100 mPa ⁇ s, and preferably 1 to 50 mPa ⁇ s. Is more preferable.
  • the viscosity is a value measured at a rotation speed of 20 rpm using an E-type digital viscometer based on JIS Z 8803: 1991 “Solution viscosity-Measurement method”.
  • the solid concentration of the p-type impurity diffusion composition of the present invention is not particularly limited, but 1% by mass to 10% by mass is a preferable range. This is because in this concentration range, the storage stability is particularly good, and the film thickness during coating is easy to control, so that adjustment to obtain a desired diffusion concentration is easy.
  • a method of manufacturing a semiconductor device according to the present invention comprises a step of applying a p-type impurity diffusion composition to a semiconductor substrate to form a p-type impurity diffusion composition film, and a step of forming a p-type impurity diffusion composition film from the p-type impurity diffusion composition film.
  • a method for manufacturing a semiconductor device which comprises the step of diffusing the semiconductor substrate into the semiconductor substrate to form a p-type impurity diffusion layer in the semiconductor substrate.
  • the p-type impurity diffusion composition film is formed by applying the p-type impurity diffusion composition of the present invention and then volatilizing the organic solvent (b-1) and the water (b-2) contained in the solvent (b). It is a film and has been described as a coating film in the use mode of the p-type impurity diffusion composition described above.
  • (b-1) the organic solvent and (b) contained in the solvent (b).
  • An operation of volatilizing water is included (hereinafter, "application and formation” means an operation of volatilizing a solvent after application.
  • the p-type impurity diffusion composition film includes “p-type impurity diffusion composition” in the name, but (b) is less solvent than the p-type impurity diffusion composition of the present invention, Alternatively, the composition is different in that (b) the solvent is not included.
  • a small amount of solvent means a state in which the solvent (b) is removed to such an extent that the coating film (p-type impurity diffusion composition film) does not flow.
  • the n-type impurity diffusion composition film is formed by partially coating the semiconductor substrate with the n-type impurity diffusion composition film and then using the n-type impurity diffusion composition film as a mask.
  • a method of manufacturing a semiconductor device including a step of applying a p-type impurity diffusion composition to a portion where the n-type impurity diffusion composition is not applied to form a p-type impurity diffusion composition film.
  • the n-type impurity diffusion composition film may be heated to form the n-type impurity diffusion layer before applying the p-type impurity diffusion composition, or the n-type and p-type impurity diffusion composition films may be formed.
  • the n-type impurity diffusion layer and the p-type impurity diffusion layer may be simultaneously formed by heating at once.
  • the n-type impurity diffusion composition is for forming an n-type impurity diffusion layer in a semiconductor substrate by containing an n-type impurity diffusion component in the composition.
  • the n-type impurity diffusion component is preferably a compound containing a Group 15 element, and more preferably a phosphorus compound.
  • phosphorus compounds include diphosphorus pentoxide, phosphoric acid, polyphosphoric acid, methyl phosphate, dimethyl phosphate, trimethyl phosphate, ethyl phosphate, diethyl phosphate, triethyl phosphate, propyl phosphate, dipropyl phosphate, and phosphoric acid.
  • Phosphoric acid esters such as tripropyl, butyl phosphate, dibutyl phosphate, tributyl phosphate, phenyl phosphate, diphenyl phosphate, and triphenyl phosphate, methyl phosphite, dimethyl phosphite, trimethyl phosphite, and phosphite.
  • the method for manufacturing a semiconductor device comprises a step of forming the p-type impurity diffusion composition film by applying the above-mentioned p-type impurity diffusion composition on one surface of the semiconductor substrate, and the other step of the semiconductor substrate.
  • a step of forming an n-type impurity diffusion composition film by applying an n-type impurity diffusion composition film on the surface of the substrate, and simultaneously heating the p-type impurity diffusion composition film and the n-type impurity diffusion composition film A method of manufacturing a semiconductor device, which includes a step of forming a p-type impurity diffusion layer and an n-type impurity diffusion layer on the semiconductor substrate.
  • the method for manufacturing a semiconductor device comprises a step of applying the above-mentioned p-type impurity diffusion composition to one surface of a semiconductor substrate to form a p-type impurity diffusion composition film, and a p-type impurity diffusion composition.
  • FIG. 1 shows a method for forming an impurity diffusion layer by applying a p-type impurity diffusion composition of the present invention to a semiconductor substrate and diffusing p-type impurities from there to the semiconductor substrate.
  • a p-type impurity diffusion composition of the present invention After coating the semiconductor substrate 1 with the p-type impurity diffusion composition of the present invention, (b) the organic solvent (b-1) and (b-2) contained in the solvent. ) Water is volatilized to form the p-type impurity diffusion composition film 2.
  • the semiconductor substrate 1 is, for example, an n-type single crystal silicon having an impurity concentration of 10 15 to 10 16 atoms/cm 3 , polycrystalline silicon, and a crystalline silicon substrate in which other elements such as germanium and carbon are mixed. Is mentioned. It is also possible to use p-type crystalline silicon or a semiconductor other than silicon.
  • the semiconductor substrate 1 preferably has a thickness of 50 to 300 ⁇ m and an outer shape of a substantially quadrangle having a side of 100 to 250 mm. Further, in order to remove the slice damage and the natural oxide film, it is preferable to etch the surface with a hydrofluoric acid solution or an alkaline solution.
  • Examples of the method for applying the p-type impurity diffusion composition include a spin coating method, a screen printing method, an inkjet printing method, a slit coating method, a spray coating method, a relief printing method, an intaglio printing method, and the like.
  • the applied p-type impurity diffusion composition is heated in a range of 50 to 200° C. for 30 seconds to 30 minutes with a hot plate, an oven or the like (b) a solvent
  • the organic solvent (b-1) and the water (b-2) contained in are volatilized and dried.
  • the film thickness of the p-type impurity diffusion composition film 2 obtained after drying is preferably 100 nm or more from the viewpoint of diffusivity of p-type impurities into the semiconductor substrate 1, and preferably 3 ⁇ m or less from the viewpoint of residues after etching.
  • p-type impurities are diffused in the semiconductor substrate 1 to form a p-type impurity diffusion layer 3.
  • a known method for diffusing the p-type impurity into the semiconductor substrate a known method by thermal diffusion can be used, and for example, methods such as electric heating, infrared heating, laser heating, and microwave heating can be used.
  • the time and temperature of thermal diffusion can be appropriately set so that desired diffusion characteristics such as the concentration of p-type impurities and the diffusion depth of p-type impurities in the obtained p-type impurity diffusion layer can be obtained.
  • desired diffusion characteristics such as the concentration of p-type impurities and the diffusion depth of p-type impurities in the obtained p-type impurity diffusion layer can be obtained.
  • a p-type diffusion layer having a surface impurity concentration of 10 19 to 10 21 can be formed.
  • the diffusion atmosphere is not particularly limited and may be performed in the air, or the amount of oxygen in the atmosphere may be appropriately controlled by using an inert gas such as nitrogen or argon. From the viewpoint of shortening the diffusion time, the oxygen concentration in the atmosphere is preferably 3% or less. Further, if necessary, heating may be performed in the range of 200° C. to 850° C. before diffusion.
  • the p-type impurity diffusion composition film 2 formed on the surface of the semiconductor substrate 1 is removed by a known etching method.
  • the material used for etching is not particularly limited, but for example, one containing at least one of hydrogen fluoride, ammonium, phosphoric acid, sulfuric acid, and nitric acid as an etching component and water and an organic solvent as the other components. preferable.
  • the p-type impurity diffusion layer can be formed on one surface of the semiconductor substrate.
  • FIG. 2 shows a step of applying an n-type impurity diffusion composition to a semiconductor substrate and diffusing n-type impurities from the n-type impurity diffusion composition into the semiconductor substrate, and using the n-type impurity diffusion composition as a mask, the semiconductor substrate And a step of applying a p-type impurity and diffusing the same, and a method of forming an impurity diffusion layer.
  • FIG. 3 illustrates a method of manufacturing a semiconductor device using the impurity diffusion layer obtained by using the process shown in FIG. 2 by taking a method of manufacturing a back junction solar cell as an example.
  • the n-type impurity diffusion composition film 4 is patterned on the semiconductor substrate 1.
  • Examples of the method for forming the n-type impurity diffusion composition film 4 include a screen printing method, an inkjet printing method, a slit coating method, a spray coating method, a relief printing method, an intaglio printing method, and the like. After applying the n-type impurity diffusion composition by these methods, the applied n-type impurity diffusion composition is dried at 50 to 200° C. for 30 seconds to 30 minutes by a hot plate, an oven or the like to diffuse the n-type impurity diffusion.
  • the composition film 4 is preferable.
  • the film thickness of the obtained n-type impurity diffusion composition film 4 is preferably 200 nm or more in view of maskability against p-type impurities, and is preferably 5 ⁇ m or less from the viewpoint of crack resistance.
  • the n-type impurities in the n-type impurity diffusion composition film 4 are diffused into the semiconductor substrate 1 to form the n-type impurity diffusion layer 5.
  • a known thermal diffusion method can be used, and, for example, a method such as electric heating, infrared heating, laser heating, or microwave heating can be used.
  • the time and temperature of thermal diffusion can be appropriately set so that desired diffusion characteristics such as the concentration of n-type impurities and the diffusion depth of n-type impurities in the obtained n-type impurity diffusion layer can be obtained. For example, by heating and diffusing at 800° C. or more and 1200° C. or less for 1 to 120 minutes, an n-type diffusion layer having a surface impurity concentration of 10 19 to 10 21 can be formed.
  • the diffusion atmosphere is not particularly limited, and it may be performed in the air, or the amount of oxygen in the atmosphere may be appropriately controlled by using an inert gas such as nitrogen or argon. From the viewpoint of shortening the diffusion time, it is preferable that the oxygen concentration in the atmosphere is 3% or less. Further, if necessary, heating may be performed in the range of 200° C. to 850° C. before diffusion.
  • the n-type impurity diffusion composition film 4 is heated if necessary, and then, as shown in FIG. A type impurity diffusion composition is applied.
  • the p-type impurity diffusion composition film 2 may be formed on the entire surface, or may be formed only on the portion where the n-type impurity diffusion composition film 4 is not present. .
  • the p-type impurity diffusion composition film 2 when the p-type impurity diffusion composition film 2 is formed on the entire surface, part of the p-type impurity diffusion composition film 2 overlaps the n-type impurity diffusion composition film 4. However, there is no particular problem.
  • Examples of the method for applying the p-type impurity diffusion composition include a spin coating method, a screen printing method, an inkjet printing method, a slit coating method, a spray coating method, a relief printing method, an intaglio printing method, and the like.
  • the applied p-type impurity diffusion composition is dried at 50 to 200° C. for 30 seconds to 30 minutes by a hot plate, an oven or the like to diffuse the p-type impurity diffusion. It is preferable to form the composition film 2.
  • the film thickness of the obtained p-type impurity diffusion composition film 2 is preferably 100 nm or more from the viewpoint of diffusivity of p-type impurities, and preferably 3 ⁇ m or less from the viewpoint of residues after etching.
  • the p-type impurity diffusion composition is diffused from the p-type impurity diffusion composition film 2 to the semiconductor substrate 1 using the heated n-type impurity diffusion composition film 4 as a mask layer.
  • P-type impurity diffusion layer 3 is formed.
  • a known thermal diffusion method can be used, and for example, methods such as electric heating, infrared heating, laser heating, and microwave heating can be used.
  • the time and temperature of thermal diffusion can be appropriately set so that desired diffusion characteristics such as the diffusion concentration of p-type impurities and the diffusion depth of p-type impurities in the obtained p-type impurity layer can be obtained.
  • a p-type diffusion layer having a surface impurity concentration of 10 19 to 10 21 can be formed by performing heat diffusion at 800° C. to 1200° C. for 1 to 120 minutes.
  • the diffusion atmosphere is not particularly limited, and it may be performed in the air, or the amount of oxygen in the atmosphere may be appropriately controlled by using an inert gas such as nitrogen or argon. From the viewpoint of shortening the diffusion time, it is preferable that the oxygen concentration in the atmosphere is 3% or less. Further, if necessary, heating may be performed in the range of 200° C. to 850° C. before diffusion.
  • the n-type impurity diffusion composition film 4 and the p-type impurity diffusion composition film 2 formed on the surface of the semiconductor substrate 1 are removed by a known etching method.
  • the material used for etching is not particularly limited, but for example, one containing at least one of hydrogen fluoride, ammonium, phosphoric acid, sulfuric acid, and nitric acid as an etching component and water or an organic solvent as the other components. preferable.
  • the p-type impurity diffusion composition is applied and diffused after the application and diffusion of the n-type impurity diffusion composition. It is also possible to apply/diffuse the diffusion composition.
  • FIG. 3F a method for manufacturing a semiconductor element of the present invention will be described by taking a back junction solar cell as an example.
  • the n-type impurity diffusion layer 5 and the p-type impurity diffusion layer 3 of the semiconductor substrate 9 having the n-type impurity diffusion layer 5 and the p-type impurity diffusion layer 3 formed on one surface are formed.
  • the protective film 6 is formed on the entire surface of the formed surface.
  • the surface on which the n-type impurity diffusion layer 5 and the p-type impurity diffusion layer 3 are formed may be referred to as the back surface.
  • the protective film 6 is patterned by an etching method or the like to form a protective film opening 6a. Further, as shown in FIG. 3(h), the n-type contact electrode 8 and the p-type contact electrode 8 are formed by pattern-coating an electrode paste on a region including the opening 6a by a stripe coating method, a screen printing method, or the like and heating it. Form 7. Thereby, the back contact solar cell 10 is obtained.
  • FIG. 4 shows a step of forming a pattern using an n-type impurity diffusion composition, a step of applying a p-type impurity diffusion composition using the n-type impurity diffusion composition as a mask, the n-type impurity diffusion composition and
  • FIG. 3 shows a method for forming an impurity diffusion layer including a step of diffusing n-type and p-type impurities into the semiconductor substrate from a p-type impurity diffusion composition.
  • the n-type impurity diffusion composition film 4 is patterned on the semiconductor substrate 1.
  • the p-type impurity diffusion composition film 2 is formed using the n-type impurity diffusion composition film 4 as a mask. Form.
  • the n-type impurity in the n-type impurity diffusion composition film 4 and the p-type impurity in the p-type impurity diffusion composition film 2 are simultaneously diffused into the semiconductor substrate 1.
  • N-type impurity diffusion layer 5 and p-type impurity diffusion layer 3 are formed.
  • the n-type impurity diffusion composition film 4 and the p-type impurity diffusion composition film 2 formed on the surface of the semiconductor substrate 1 are removed by a known etching method.
  • the n-type and p-type impurity diffusion layers can be formed on one surface of the semiconductor substrate.
  • the p-type impurity diffusion composition film 2 of the present invention is formed on the semiconductor substrate 1. After heating the p-type impurity diffusion composition film 2 as needed, as shown in FIG. 5B, the surface of the semiconductor substrate 1 opposite to the surface on which the p-type impurity diffusion composition film 2 is formed. Then, the n-type impurity diffusion composition film 4 is formed.
  • p-type impurities from the p-type impurity diffusion composition film 2 and n-type impurities from the n-type impurity diffusion composition film 4 are simultaneously diffused into the semiconductor substrate 1, A p-type impurity diffusion layer 3 and an n-type impurity diffusion layer 5 are formed.
  • Examples of the method of applying the n-type and p-type impurity diffusion composition, the method of heating, and the method of diffusion include the same methods as those described above with reference to FIG.
  • the p-type impurity diffusion composition film 2 and the n-type impurity diffusion composition film 4 formed on the surface of the semiconductor substrate 1 are removed by a known etching method.
  • n-type and p-type impurity diffusion layers can be formed on the semiconductor substrate.
  • the p-type impurity diffusion composition is applied and then the n-type impurity diffusion composition is applied is shown.
  • the p-type impurity diffusion composition is applied. Is also possible.
  • the p-type impurity diffusion composition film 2 of the present invention is formed on the semiconductor substrate 1.
  • a pair of two semiconductor substrates having the p-type impurity diffusion composition film 2 formed thereon are arranged such that the surfaces having the p-type impurity diffusion composition film 2 face each other. Arrange so that they fit together.
  • the distance between the facing surfaces is preferably 5 mm or less, and more preferably in contact with each other.
  • p-type impurities are diffused from the p-type impurity diffusion composition film 2 into the semiconductor substrate 1 to form the p-type impurity diffusion layer 3.
  • the method of applying the p-type impurity diffusion composition the method of heating, and the method of diffusion, the same methods as those described above based on FIG. 1 can be mentioned.
  • the semiconductor substrate is continuously and continuously exposed to an atmosphere containing a gas containing n-type impurities. 1 is heated to form the n-type impurity diffusion layer 5 on the surface of the semiconductor substrate 1 on which the p-type impurity diffusion composition film 2 is not formed.
  • the semiconductor substrate 1 may be heated in an atmosphere containing oxygen to form an oxide film on the semiconductor substrate 1.
  • the oxide film remaining in 5 is removed.
  • the p-type impurity diffusion composition of the present invention is applied to a photovoltaic device such as a solar cell and a semiconductor device in which an impurity diffusion region is patterned on a semiconductor surface, such as a transistor array, a diode array, a photodiode array and a transducer. Can also be deployed.
  • the viscosity immediately after preparation of the p-type impurity diffusion composition and the viscosity after preparation for 30 days after storage at 25° C. and after storage for 30 days at 3° C. were measured. Those that passed or exceeded 20% were rejected.
  • a 6-inch silicon wafer (manufactured by Electronics End Materials Corporation) is immersed in a 1% aqueous solution of hydrofluoric acid for 1 minute, washed with water, blown with air, and heated at 140° C. on a hot plate at 5° C. Processed for minutes.
  • the p-type impurity diffusion composition was applied to the silicon wafer by spin coating so that the thickness of the coating film was 1 ⁇ m. After coating, the silicon wafer was heated at 140° C. for 5 minutes.
  • the heated wafer was measured at 15 points at equal intervals in the diameter direction, and those having a (maximum value-minimum value) value of 0.3 ⁇ m or less were accepted, and those exceeding 0.3 ⁇ m were rejected.
  • Sheet resistance uniformity impurity diffusion concentration uniformity
  • the p-type impurity diffusion composition was applied to the silicon wafer by spin coating so that the thickness of the coating film was about 500 nm. After coating, the silicon wafer was heated at 140° C. for 5 minutes.
  • the p/n judgment machine is used for p/n judgment on the peeled silicon wafer, and the surface resistance is measured in the direction using a four-probe surface resistance measuring device RT-70V (manufactured by Napson Corporation).
  • the p-type impurity diffusion composition was applied to the silicon wafer by spin coating so that the thickness of the coating film was about 2 ⁇ m. After coating, the silicon wafer was heated at 140° C. for 5 minutes.
  • each silicon wafer was immersed in a 5 mass% hydrofluoric acid aqueous solution at 23° C. for 1 minute to peel off the composition. After the peeling, the silicon wafer was immersed in pure water for cleaning, and the presence or absence of a residue was visually observed on the surface. After 1 minute of immersion, surface deposits can be visually confirmed and cannot be removed by rubbing with a waste cloth, but after further dipping for 5 minutes, those that can be removed by rubbing with a waste cloth are visible. It can be confirmed, but it can be removed by rubbing with a waste cloth C, it is more than 30 seconds and the surface deposit can not be visually confirmed within 1 minute, B is the surface deposit can not be visually confirmed within 30 seconds Was designated as A. From the viewpoint of suppressing the organic residue, it can be judged that the preferable result is in the order of D ⁇ C ⁇ B ⁇ A.
  • Formulation example 1 A 150 mL three-necked flask was charged with 4.21 g of PVA (JP-03, manufactured by Japan Vine & Hoval Co., Ltd.) and 14.2 g of water, heated to 80° C. with stirring and stirred for 1 hour, and then 1 -BuOH (manufactured by Tokyo Kasei Co., Ltd.) 80.3 g and boric acid (manufactured by Fuji Yakuhin Kogyo Co., Ltd.) 1.29 g were added, and the mixture was stirred at 80° C. for 1 hour.
  • PVA JP-03, manufactured by Japan Vine & Hoval Co., Ltd.
  • 1 -BuOH manufactured by Tokyo Kasei Co., Ltd.
  • boric acid manufactured by Fuji Yakuhin Kogyo Co., Ltd.
  • a silicone surfactant BYK333 manufactured by BYK Japan KK was added, and the mixture was stirred for 30 minutes.
  • This mixed solution was treated by ion exchange treatment A and then filtered through a 20 ⁇ m filter to obtain a p-type impurity diffusion composition A.
  • the composition thus obtained had a viscosity of 18 mPa ⁇ s and a pH of 5.0.
  • Formulation Examples 2-23 The compositions shown in Table 1 were mixed, ion-exchanged and filtered through a 20 ⁇ m filter in the same manner as in Formulation Example 1 to obtain p-type impurity diffusion compositions B to X. However, in the formulation examples 16, 21, 22, and 23, the ion exchange treatment was not performed. In addition, in Formulation Examples 15, 16, 21, and 22, an organic base or an acid was further added.
  • the ion exchange treatment was performed by either of the following methods (A) and (B).
  • A) The mixed solution containing the respective components is passed through a column packed with a cation exchange resin (Amberlyst 15JS-HG-DRY manufactured by Organo Corporation).
  • B) The mixed solution containing the respective components is passed through a column packed with a cation/anion mixed exchange resin (Amberlyst MSPS2-1-DRY manufactured by Organo Corporation).
  • (d)/(c) ( ⁇ 1) means “(d) surfactant/(c) mass ratio of group 13 element compound” to “(c)/(a)” ( ⁇ 2) represents “(c) Group 13 element compound/(a) resin mass ratio”.

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Abstract

Le but de la présente invention est de pourvoir à une composition pour diffusion d'impuretés du type p qui permette de réaliser une dispersion uniforme sur un substrat semi-conducteur et d'augmenter la stabilité au stockage d'un liquide de revêtement. Cette composition pour diffusion d'impuretés du type p contient (a) au moins une résine choisie parmi le poly(alcool vinylique) et le poly(oxyde d'éthylène), (b) un solvant, et (c) un composé contenant un élément du groupe 13, et est caractérisée en ce que le pH de la composition est de 4 à 6,5, le solvant (b) contient (b-1) un solvant organique ayant un point d'ébullition de 110 à 210 °C et (b-2) de l'eau, et la quantité d'eau (b-2) est de 10 à 50 % en masse du solvant (b).
PCT/JP2019/046319 2018-12-07 2019-11-27 Composition pour diffusion d'impuretés du type p et son procédé de production, procédé de fabrication d'élément à semi-conducteur utilisant ladite composition pour diffusion, et batterie solaire Ceased WO2020116270A1 (fr)

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JP2019565963A JP7463725B2 (ja) 2018-12-07 2019-11-27 ｐ型不純物拡散組成物とその製造方法、それを用いた半導体素子の製造方法および太陽電池

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JP2020194827A (ja) * 2019-05-24 2020-12-03 東京応化工業株式会社 拡散剤組成物、及び半導体基板の製造方法
JP2023545996A (ja) * 2020-10-22 2023-11-01 マイヤー ブルガー （ジャーマニー）ゲーエムベーハー 光起電力デバイス及びその製造方法
JP7782635B1 (ja) 2024-09-19 2025-12-09 栗田工業株式会社 半導体基板のドーピング処理方法およびドーピング処理装置
JP7782749B1 (ja) 2024-09-19 2025-12-09 栗田工業株式会社 調整水の製造装置および調整水の製造方法
JP7782636B1 (ja) 2024-09-19 2025-12-09 栗田工業株式会社 調整水の製造装置および調整水の製造方法

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WO2018021117A1 (fr) * 2016-07-26 2018-02-01 東レ株式会社 Procédé de production d'éléments semi-conducteurs et procédé de production de cellules solaires
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JP2014030011A (ja) * 2012-07-04 2014-02-13 Nippon Synthetic Chem Ind Co Ltd:The ドーパント拡散用塗布液、およびその塗布方法、並びにそれを用いた半導体の製法、半導体
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JP2020194827A (ja) * 2019-05-24 2020-12-03 東京応化工業株式会社 拡散剤組成物、及び半導体基板の製造方法
JP7428478B2 (ja) 2019-05-24 2024-02-06 東京応化工業株式会社 拡散剤組成物、及び半導体基板の製造方法
JP2023545996A (ja) * 2020-10-22 2023-11-01 マイヤー ブルガー （ジャーマニー）ゲーエムベーハー 光起電力デバイス及びその製造方法
JP7782635B1 (ja) 2024-09-19 2025-12-09 栗田工業株式会社 半導体基板のドーピング処理方法およびドーピング処理装置
JP7782749B1 (ja) 2024-09-19 2025-12-09 栗田工業株式会社 調整水の製造装置および調整水の製造方法
JP7782636B1 (ja) 2024-09-19 2025-12-09 栗田工業株式会社 調整水の製造装置および調整水の製造方法

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