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WO2016010095A1 - Procédé de fabrication de substrat semi-conducteur comprenant une couche de diffusion de type n, et procédé de fabrication d'élément de cellule solaire - Google Patents

Procédé de fabrication de substrat semi-conducteur comprenant une couche de diffusion de type n, et procédé de fabrication d'élément de cellule solaire Download PDF

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Publication number
WO2016010095A1
WO2016010095A1 PCT/JP2015/070322 JP2015070322W WO2016010095A1 WO 2016010095 A1 WO2016010095 A1 WO 2016010095A1 JP 2015070322 W JP2015070322 W JP 2015070322W WO 2016010095 A1 WO2016010095 A1 WO 2016010095A1
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Prior art keywords
diffusion layer
type diffusion
semiconductor substrate
type
manufacturing
Prior art date
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PCT/JP2015/070322
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English (en)
Japanese (ja)
Inventor
岩室　光則
野尻　剛
倉田　靖
芦沢　寅之助
明博 織田
麻理 清水
鉄也 佐藤
佐藤　英一
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Resonac Corp
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Hitachi Chemical Co Ltd
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Priority to CN201580038703.6A priority Critical patent/CN106537559A/zh
Priority to JP2016534479A priority patent/JPWO2016010095A1/ja
Publication of WO2016010095A1 publication Critical patent/WO2016010095A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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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
    • H10F10/14—Photovoltaic cells having only PN homojunction potential barriers
    • 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 method for manufacturing a semiconductor substrate having an n-type diffusion layer and a method for manufacturing a solar cell element.
  • the crystalline silicon solar cell element is a power generation element including a p-type semiconductor region and an n-type semiconductor region.
  • a p-type semiconductor region or an n-type semiconductor region is formed on the whole or part of the crystalline silicon substrate.
  • p-type such as boron or aluminum used for forming the p-type semiconductor region.
  • barrier layer it is common to use a silicon oxide film that does not decompose even when subjected to a high-temperature treatment and can be removed by dissolving with hydrofluoric acid when unnecessary.
  • a method for forming a silicon oxide film a dry oxidation method or a wet oxidation method is often used.
  • a silicon oxide film is formed by these silicon oxide film forming methods, a thick silicon oxide film is selectively formed on the n-type semiconductor region (see, for example, JP-A-2014-86587).
  • the barrier layer protecting the n-type semiconductor region needs to be thick so that p-type dopants such as boron and aluminum used to form the p-type semiconductor do not diffuse into the n-type semiconductor region. .
  • p-type dopants such as boron and aluminum used to form the p-type semiconductor do not diffuse into the n-type semiconductor region.
  • the present invention has been made in view of the above circumstances, and enables an n-type diffusion layer to be formed in a desired portion of a semiconductor substrate, and a p-type dopant used for forming a p-type semiconductor is an n-type.
  • Means for solving the above problems include the following embodiments.
  • a method for manufacturing a semiconductor substrate having an n-type diffusion layer comprising a step of heat-treating under conditions that are seconds.
  • ⁇ 3> The method for producing a semiconductor substrate having an n-type diffusion layer according to ⁇ 1> or ⁇ 2>, wherein the donor element is at least one selected from the group consisting of P (phosphorus) and Sb (antimony) .
  • Glass particles containing the donor element are At least one donor element-containing material selected from the group consisting of P 2 O 3 , P 2 O 5 and Sb 2 O 3 , and SiO 2 , K 2 O, Na 2 O, Li 2 O, BaO, SrO, ⁇ 1> to ⁇ 3> containing at least one glass component material selected from the group consisting of CaO, MgO, BeO, ZnO, PbO, CdO, V 2 O 5 , SnO, ZrO 2 and MoO 3
  • the manufacturing method of the semiconductor substrate which has an n type diffused layer of any one of these.
  • ⁇ 5> The method for producing a semiconductor substrate having an n-type diffusion layer according to any one of ⁇ 1> to ⁇ 4>, further including a step of oxidizing the semiconductor substrate having the n-type diffusion layer.
  • ⁇ 6> Production of a semiconductor substrate having an n-type diffusion layer according to any one of ⁇ 1> to ⁇ 5>, wherein the oxidation treatment is at least one selected from the group consisting of dry oxidation and wet oxidation Method.
  • ⁇ 7> The method for producing a semiconductor substrate having an n-type diffusion layer according to any one of ⁇ 1> to ⁇ 6>, wherein the semiconductor substrate is a silicon substrate.
  • n-type diffusion layer in a desired portion of a semiconductor substrate and prevent the p-type dopant used for forming the p-type semiconductor from diffusing into the n-type semiconductor region.
  • a method for manufacturing a semiconductor substrate having an n-type diffusion layer and a method for manufacturing a solar cell element which can form a barrier layer and reduce variation in sheet resistance.
  • the present invention will be described in detail. However, the present invention is not limited to the following embodiments.
  • the constituent elements including element steps and the like) are not essential unless explicitly specified, unless otherwise clearly considered essential in principle.
  • the term “process” includes a process that is independent of other processes and includes the process if the purpose of the process is achieved even if it cannot be clearly distinguished from the other processes. It is.
  • numerical values indicated by using “to” include numerical values described before and after “to” as the minimum value and the maximum value, respectively.
  • each component in the composition is the sum of the plurality of substances present in the composition unless there is a specific indication when there are a plurality of substances corresponding to each component in the composition. It means the content rate of.
  • the particle diameter of each component in the composition is a mixture of the plurality of types of particles present in the composition unless there is a specific indication when there are a plurality of types of particles corresponding to each component in the composition. Means the value of.
  • the term “layer” refers to the case where the layer is formed only in a part of the region in addition to the case where the layer is formed over the entire region. Is also included.
  • the method for manufacturing a semiconductor substrate having an n-type diffusion layer includes an n-type diffusion layer forming composition containing glass particles containing a donor element and a dispersion medium (hereinafter referred to as “specific n-type diffusion layer formation”).
  • the method for manufacturing a semiconductor substrate having an n-type diffusion layer may further include other steps as necessary.
  • linear velocity in the heat treatment step means a distance that the gas travels per unit time.
  • the value of the linear velocity is a value that does not depend on the conditions of the diffusion furnace to be used (for example, the design value (diameter) of the quartz tube). For example, when the diameter of the quartz tube of the diffusion furnace is 252 mm and the linear velocity is 10 mm / second, the flow rate per unit time is obtained by multiplying the cross-sectional area calculated from the diameter of the quartz tube by the linear velocity. In this case, 30 L of gas flows in the quartz tube per minute. If the linear velocity is 3 mm / second or 60 mm / second with the diameter of the quartz tube made of 252 mm, the gas flow rate is 9 L / min or 180 L / min, respectively.
  • the manufacturing method of a semiconductor substrate having an n-type diffusion layer can form an oxide film having a sufficient thickness as a barrier layer that prevents the p-type dopant from diffusing into the n-type semiconductor region by having the above structure. .
  • the reason is not clear, but is presumed as follows.
  • the specific n-type diffusion layer forming composition contains glass particles containing a donor element and a dispersion medium. Glass particles soften at high temperatures during heat treatment. The donor element moves from the softened glass particles to the semiconductor substrate to form an n-type semiconductor region, and a glass layer is formed on the n-type semiconductor region by the glass component in the glass particles.
  • the n-type semiconductor region on the semiconductor substrate is exposed by removing the glass layer by etching with hydrofluoric acid or the like.
  • the exposed n-type semiconductor region is more easily oxidized than a region where the donor element is not diffused. Therefore, by performing the oxidation treatment, an oxide film is formed thicker on the n-type semiconductor region than the region where the donor element is not diffused. This oxide film functions as a barrier film when the p-type dopant is diffused in a later step.
  • the gas flow rate to 3 mm / second to 60 mm / second, the dispersion medium contained in the n-type diffusion layer forming composition is efficiently scattered and the glass layer is easily formed. Furthermore, the residual ratio of the dispersion medium in the glass layer to be formed can be reduced, and variations in sheet resistance of the manufactured semiconductor substrate and solar cell element having the n-type diffusion layer are reduced.
  • n-type diffusion layer forming composition a specific n-type diffusion layer forming composition will be described, and then a semiconductor substrate manufacturing method and a solar cell element manufacturing method using these n-type diffusion layer forming compositions will be described.
  • the specific n-type diffusion layer forming composition contains glass particles containing a donor element (hereinafter also referred to as “glass particles”) and a dispersion medium.
  • the specific n-type diffusion layer forming composition may contain other components as required in consideration of coating properties and the like.
  • the n-type diffusion layer forming composition contains a donor element, and is applied to the semiconductor substrate, and then thermally diffuses the donor element, so that the n-type diffusion layer forming composition of the semiconductor substrate is applied to the site.
  • an n-type diffusion layer can be selectively formed in a desired portion of the semiconductor substrate to which the specific n-type diffusion layer forming composition is applied, and on the back surface, side surface, etc. of the semiconductor substrate It becomes easy not to form an unnecessary n-type diffusion layer. Therefore, if the specific n-type diffusion layer forming composition is applied, the side etching step performed by the gas phase reaction method that has been widely adopted conventionally becomes unnecessary, and the process tends to be simplified. Further, there is no need to convert the n-type diffusion layer formed on the back surface of the semiconductor substrate into a p + -type diffusion layer.
  • the method for forming the p + -type diffusion layer on the back surface, the material, shape, thickness, and the like of the back electrode are not limited, and options for the manufacturing method, material, shape, and the like to be applied are expanded. Moreover, although mentioned later for details, generation
  • the glass particles contained in the specific n-type diffusion layer forming composition are melted by heat treatment to form a glass layer on the n-type diffusion layer.
  • a glass layer is formed on the n-type diffusion layer even in a conventional gas phase reaction method, a method of applying a phosphate-containing solution, or the like. Therefore, the glass layer formed in the method of the present embodiment can be removed by etching as in the conventional method. Therefore, the specific n-type diffusion layer forming composition tends not to generate unnecessary products and increase the number of steps as compared with the conventional method.
  • the glass particles are not volatilized even during the heat treatment, the generation of the volatilized gas tends to prevent the n-type diffusion layer from being formed not only on the surface of the semiconductor substrate but also on the back surface or side surface of the semiconductor substrate. For this reason, for example, it is considered that the donor component is not easily volatilized because it is bonded to the element in the glass particle or is taken into the glass.
  • the donor element contained in the glass particles means an element that can be diffused into the semiconductor substrate by doping to form an n-type diffusion layer.
  • a Group 15 element can be used.
  • the Group 15 element include P (phosphorus), Sb (antimony), and As (arsenic). From the viewpoint of safety, ease of vitrification, etc., the donor element is preferably at least one selected from the group consisting of P (phosphorus) and Sb (antimony).
  • Examples of the donor element-containing material used for introducing the donor element into the glass particles include P 2 O 3 , P 2 O 5 , Sb 2 O 3 , Bi 2 O 3 , and As 2 O 3. At least one selected from the group consisting of 2 O 3 , P 2 O 5 and Sb 2 O 3 is preferable.
  • the glass particles can be controlled in terms of melting temperature, softening point, glass transition point, chemical durability, and the like by adjusting the component ratio as necessary. From this viewpoint, it is preferable that the glass particles further contain a glass component substance as described below.
  • the glass component material include SiO 2 , K 2 O, Na 2 O, Li 2 O, BaO, SrO, CaO, MgO, BeO, ZnO, PbO, CdO, SnO, WO 3 , MoO 3 , MnO, and La. 2 O 3 , Nb 2 O 5 , Ta 2 O 5 , Y 2 O 3 , TiO 2 , ZrO 2 , GeO 2 , TeO 2 , and Lu 2 O 3 may be mentioned.
  • the glass particles are made of SiO 2 , K 2 O, Na 2 O, Li 2 O, BaO, SrO, CaO, MgO, BeO, ZnO, PbO, CdO, SnO, ZrO 2 , WO 3 , MoO 3 and MnO. It is preferable to include at least one selected from the glass component substances.
  • the glass particles are composed of SiO 2 , K 2 O, Na 2 O, Li 2 O, BaO, SrO, CaO, MgO, BeO, ZnO, PbO, CdO, V 2 O 5 , SnO, ZrO 2 and MoO 3. It is more preferable that at least one selected from the above is included as a glass component substance.
  • the glass particles containing a donor element include at least one donor element-containing material selected from the group consisting of P 2 O 3 , P 2 O 5 and Sb 2 O 3 , and SiO 2 , K 2 O. , Na 2 O, Li 2 O, BaO, SrO, CaO, MgO, BeO, ZnO, PbO, CdO, V 2 O 5 , SnO, ZrO 2, and MoO 3. It is preferable to contain a substance.
  • the glass particles containing a donor element in the present invention include, for example, P 2 O 5 —SiO 2 glass particles, P 2 O 5 —K 2 O glass particles, and P 2 O 5 —Na 2 O glass.
  • the glass particles may be composite glass particles containing three or more kinds of components such as P 2 O 5 —SiO 2 —CaO as desired.
  • the content of the glass component substance in the glass particles is desirably set as appropriate in consideration of the melting temperature, softening point, glass transition point, chemical durability, and the like.
  • the content of the glass component substance is preferably 0.1% by mass to 95% by mass, and more preferably 0.5% by mass to 90% by mass.
  • the softening point of the glass particles is preferably 200 ° C. to 1000 ° C., for example, from 300 ° C. to 900 ° C. from the viewpoint of diffusibility of the components of the specific n-type diffusion layer forming composition during heat treatment, dripping, etc. It is more preferable that
  • the shape of the glass particles examples include a substantially spherical shape, a flat shape, a block shape, a plate shape, and a scale shape.
  • the glass particles are preferably substantially spherical, flat or plate-like from the viewpoint of application properties to a semiconductor substrate, uniform diffusibility, and the like when an n-type diffusion layer forming composition is used.
  • the average particle size of the glass particles is preferably 100 ⁇ m or less, for example. When glass particles having an average particle size of 100 ⁇ m or less are used, a smooth composition layer is easily obtained.
  • the average particle size of the glass particles is, for example, preferably 50 ⁇ m or less, and more preferably 30 ⁇ m or less.
  • the lower limit is not particularly limited, but is preferably 0.01 ⁇ m or more, for example.
  • the average particle diameter of the glass particles represents a volume average particle diameter, and can be measured by a laser scattering diffraction particle size distribution measuring apparatus or the like.
  • the volume average particle diameter is a value (D 50 ) when the accumulation from the small diameter side is 50% in the volume-based particle diameter distribution.
  • Glass particles containing a donor element can be produced by the following procedure.
  • a glass particle raw material containing a donor element is weighed and filled in a crucible.
  • the material for the crucible include platinum, platinum-rhodium, gold, iridium, alumina, quartz, carbon, and the like, which are appropriately selected in consideration of the melting temperature, atmosphere, reactivity with the molten material, and the like.
  • it heats with the temperature according to a glass composition with an electric furnace, and is set as a melt. At this time, it is desirable to stir so that the melt is sufficiently mixed.
  • the heating temperature is not particularly limited as long as it is a temperature at which the donor element-containing material is combined with the glass component material.
  • the glass component substance when SiO 2 is used as the glass component substance, it is preferable to produce a glass particle containing the donor element by heating a mixture containing the glass component substance and the donor element-containing substance to 1400 ° C. or higher. Subsequently, the obtained melt is poured onto a metal plate or the like to vitrify the melt. Next, the obtained glass is pulverized into particles.
  • a known method using a stamp mill, a jet mill, a bead mill, a ball mill or the like can be applied.
  • the content ratio of the glass particles containing the donor element in the n-type diffusion layer forming composition is determined in consideration of the coating property, the diffusibility of the donor element, and the like.
  • the glass particle content in the n-type diffusion layer forming composition is, for example, 0.1% by mass to 95% by mass with respect to the total mass of the n-type diffusion layer forming composition. It is preferably 1% by mass to 90% by mass, more preferably 2% by mass to 80% by mass.
  • the content of the glass particles containing the donor element in the n-type diffusion layer forming composition is, for example, 0.1% by mass to 99% by mass with respect to the total amount of nonvolatile components in the n-type diffusion layer forming composition. It is preferably 1% by mass to 95% by mass, more preferably 2% by mass to 90% by mass.
  • the “nonvolatile component” means a component in the n-type diffusion layer forming composition other than a volatile substance such as a solvent described later.
  • the volatile substance means a substance having a boiling point of 250 ° C. or lower under atmospheric pressure.
  • the dispersion medium is a medium in which the glass particles are dispersed in the specific n-type diffusion layer forming composition.
  • a binder, a solvent, or the like is used as the dispersion medium.
  • binder examples include dimethylaminoethyl (meth) acrylate polymer, polyvinyl alcohol, polyacrylamides, polyvinylamides, polyvinylpyrrolidone, poly (meth) acrylic acids, polyethylene oxides, polysulfonic acid, acrylamide alkyl sulfonic acid, and cellulose ether.
  • Cellulose derivatives carboxymethyl cellulose, hydroxyethyl cellulose, ethyl cellulose, gelatin, starch and starch derivatives, sodium alginate, xanthan, guar gum and guar gum derivatives, scleroglucan, tragacanth, dextrin derivatives, acrylic acid resin, acrylate resin, butadiene Examples thereof include resins, styrene resins, copolymers thereof, and silicon dioxide.
  • a binder is used individually by 1 type or in combination of 2 or more types.
  • the weight average molecular weight of the binder is not particularly limited, and it is desirable to appropriately adjust in consideration of a desired viscosity as the specific n-type diffusion layer forming composition.
  • Examples of the solvent include acetone, methyl ethyl ketone, methyl-n-propyl ketone, methyl isopropyl ketone, methyl-n-butyl ketone, methyl isobutyl ketone, methyl-n-pentyl ketone, methyl-n-hexyl ketone, diethyl ketone, and dipropyl.
  • Ketone solvents such as ketone, diisobutylketone, trimethylnonanone, cyclohexanone, cyclopentanone, methylcyclohexanone, 2,4-pentanedione, acetonylacetone, ⁇ -butyrolactone, ⁇ -valerolactone, diethyl ether, methyl ethyl ether, Methyl-n-di-n-propyl ether, diisopropyl ether, tetrahydrofuran, methyltetrahydrofuran, dioxane, dimethyldioxane, ethylene glycol dimethyl ether, ethyl Lenglycol diethyl ether, ethylene glycol di-n-propyl ether, ethylene glycol dibutyl ether, diethylene glycol dimethyl ether, diethylene glycol diethyl ether, diethylene glycol methyl ethyl ether, diethylene glycol
  • the content of the dispersion medium in the specific n-type diffusion layer forming composition is determined in consideration of coating properties, donor concentration, and the like.
  • the viscosity of the specific n-type diffusion layer forming composition is, for example, preferably from 10 mPa ⁇ S to 1000000 mPa ⁇ S, and more preferably from 50 mPa ⁇ S to 500000 mPa ⁇ S, from the viewpoint of applicability.
  • the specific n-type diffusion layer forming composition may contain other additives.
  • other additives include metals.
  • the n-type diffusion layer forming composition is applied on a semiconductor substrate and heat-treated at a high temperature to form an n-type diffusion layer, and at that time, a glass layer is formed on the surface of the n-type diffusion layer. This glass layer can be removed by etching. However, it may be difficult to remove depending on the type of glass formed. In that case, the glass is removed during the etching by adding a metal such as Al, Ag, Mn, Cu, Fe, Zn, Si, which easily crystallizes with the glass layer, to the n-type diffusion layer forming composition. It tends to be easier.
  • the metal as a conductive material is not a main component, and the metal content depends on the type of glass, the type of metal, and the like. It is desirable to adjust appropriately.
  • the content of the metal in the n-type diffusion layer forming composition is 10% by mass with respect to the glass particles from the viewpoint of not reducing the bulk lifetime of the semiconductor substrate. Is preferably 7% by mass or less, more preferably 5% by mass or less.
  • the metal content is preferably 0.01% by mass or more with respect to the glass particles from the viewpoint of the glass layer removal efficiency, The content is more preferably 1% by mass or more, and further preferably 3% by mass or more.
  • the semiconductor substrate used in the present invention is not particularly limited, and a semiconductor substrate used for a solar cell element can be applied.
  • Examples include substrates, indium phosphide substrates, silicon carbide, silicon germanium substrates, and copper indium selenium substrates.
  • An example of the silicon substrate is a crystalline silicon substrate.
  • the semiconductor substrate is preferably pretreated before applying the specific n-type diffusion layer forming composition.
  • pretreatment include the following steps. In the following description, a specific n-type semiconductor substrate is used, but a p-type semiconductor substrate may be used.
  • An alkaline solution is applied to the n-type semiconductor substrate to remove the damaged layer, and a texture structure is obtained by etching. Specifically, the damaged layer on the surface of the n-type semiconductor substrate generated when slicing from the ingot is removed with a 20% by mass aqueous sodium hydroxide solution.
  • etching is performed with a mixed liquid of 1% by mass caustic soda and 10% by mass isopropyl alcohol to form a texture structure.
  • the solar cell element has a texture structure on the light receiving surface side, thereby promoting a light confinement effect and increasing efficiency.
  • the method for producing a semiconductor substrate having an n-type diffusion layer according to the present invention comprises an n-type diffusion layer forming composition (hereinafter referred to as “specific”) containing glass particles containing a donor element and a dispersion medium before the heat treatment step.
  • the n-type diffusion layer forming composition layer (hereinafter also referred to as “n-type diffusion composition layer”) is formed by applying at least part of the semiconductor substrate.
  • a step hereinafter also referred to as “n-type diffusion composition layer forming step”) may be included.
  • the method for applying the specific n-type diffusion layer forming composition to at least a part of the semiconductor substrate is not particularly limited.
  • a printing method, a spin coating method, a brush coating, a spray method, a doctor blade method, a roll coating method, and an ink jet method can be mentioned.
  • the shape of the region to which the specific n-type diffusion layer forming composition is applied can be appropriately changed depending on the region where the n-type diffusion layer is to be formed.
  • the n-type diffusion composition layer is dried to obtain a dispersion medium. You may remove at least one part.
  • the drying temperature is not particularly limited, and examples thereof include a temperature of about 80 ° C. to 300 ° C. For example, it can be dried for about 1 to 10 minutes when using a hot plate, and about 10 to 30 minutes when using a dryer or the like.
  • the drying conditions depend on the dispersion medium composition of the specific n-type diffusion layer forming composition, and are not particularly limited to the above conditions in the present invention.
  • Heat treatment process In the heat treatment step, a semiconductor substrate to which at least part of the composition for forming an n-type diffusion layer containing glass particles containing a donor element and a dispersion medium is applied at a gas flow rate of 3 mm / second to 60 mm at a linear velocity.
  • the heat treatment is performed under the condition of / sec.
  • the donor element diffuses into the n-type semiconductor substrate, and an n-type diffusion layer is formed.
  • a glass layer such as phosphate glass is formed on the surface of the n-type diffusion layer.
  • the gas flow rate in the heat treatment step is 3 mm / second or more in linear velocity, there is a tendency that a high concentration of the donor element can be diffused in the formed n-type diffusion layer. If the gas flow rate is 60 mm / sec or less in terms of linear velocity, it is easy to suppress variations in the heat treatment temperature, and a stable quality n-type diffusion layer is likely to be obtained.
  • the flow rate of the gas is, for example, preferably 4 mm / second or more, more preferably 5 mm / second or more, and 6 mm / second or more in linear velocity. Is more preferable.
  • the flow rate of the gas is, for example, preferably 50 mm / second or less, more preferably 40 mm / second or less, and further preferably 30 mm / second or less in linear velocity. It is particularly preferably 20 mm / second or less.
  • the heat treatment temperature is not particularly limited, and examples thereof include 600 ° C. to 1200 ° C. From the viewpoint of suppressing temperature variations in the heating device, the temperature is preferably 700 ° C. to 1150 ° C., more preferably 750 ° C. to 1100 ° C.
  • the heat treatment time is not particularly limited and may be, for example, 1 minute to 60 minutes, and may be 2 minutes to 40 minutes from the viewpoint of mass productivity of manufacturing a semiconductor substrate having an n-type diffusion layer and a solar cell element. Preferably, it is 3 minutes to 25 minutes.
  • the kind of gas in the heat treatment step is not particularly limited, and can be selected from a single gas, a compound gas, and the like.
  • the single gas include nitrogen gas, oxygen gas, hydrogen gas, helium gas, neon gas, argon gas, krypton gas, xenon gas, radon gas, and halogen gas.
  • the compound gas organic gases such as methane and propane, phosphorus oxychloride, boron tribromide, boron trichloride, etc. that can be gasified by heating can be used. These can be used alone or in combination of two or more.
  • the gas in the heat treatment step may contain air.
  • the gas in the heat treatment step preferably contains oxygen gas from the viewpoint of forming an n-type diffusion layer on which variation in thickness and the like is suppressed on the semiconductor substrate.
  • the mixing ratio of oxygen gas is not particularly limited in the present invention.
  • a known continuous diffusion furnace, batch diffusion furnace, or the like can be used.
  • the method for manufacturing a semiconductor substrate having an n-type diffusion layer according to the present invention further includes a step of removing the glass layer formed on the semiconductor substrate by etching after the heat treatment step (hereinafter also referred to as “etching step”). May be included.
  • etching step a step of removing the glass layer formed on the semiconductor substrate by etching after the heat treatment step.
  • the n-type semiconductor substrate can be cooled to room temperature and then etched.
  • Etching can be performed by a known method such as a method of immersing in an acid such as hydrofluoric acid or a method of immersing in an alkali such as caustic soda.
  • the glass layer formed on the surface of the n-type diffusion layer by the heat treatment step is formed by melting the glass particles at the above heat treatment temperature and cooling it.
  • the cooling rate is preferably in the range of 5 ° C./second to 300 ° C./second, for example.
  • the cooling rate is 300 ° C./second or less, the surface of the glass layer is suppressed from being cooled more rapidly than the other parts, and the decrease in the cooling rate inside the glass layer is suppressed. Generation is easily suppressed.
  • the cooling rate is more preferably 10 ° C./second to 50 ° C./second.
  • the n-type semiconductor substrate may be washed and dried.
  • the method for manufacturing a semiconductor substrate having an n-type diffusion layer may further include a step of oxidizing the semiconductor substrate having the n-type diffusion layer (hereinafter also referred to as “oxidation processing step”).
  • An oxide film such as a silicon oxide film is formed by the oxidation treatment.
  • the oxide film tends to be formed thick in the region of the n-type diffusion layer and thin in other regions.
  • the oxide film other than the region of the n-type diffusion layer is preferably removed by etching. At that time, the thickness of the oxide film formed in the region of the n-type diffusion layer also tends to be reduced by etching.
  • the method for the oxidation treatment is not particularly limited, and is preferably at least one selected from the group consisting of dry oxidation and wet oxidation.
  • Dry oxidation means an oxidation method by treating at a high temperature in an oxygen gas atmosphere. Dry oxidation conditions are not particularly limited, and for example, it is preferable to perform the treatment at 800 ° C. to 1100 ° C. for 10 minutes to 240 minutes.
  • Wet oxidation means an oxidation method by processing at a high temperature using oxygen gas and deionized water vapor.
  • the conditions for wet oxidation are not particularly limited. For example, it is preferable to perform the treatment at 800 ° C. to 1100 ° C. for 10 minutes to 240 minutes.
  • a step of diffusing a p-type donor element may be further included after the oxidation treatment step.
  • a p-type donor element source for example, a gas containing a p-type donor element such as boron tribromide (BBr 3 ) or boron trichloride (BCl 3 ), and other components such as a p-type donor element and a dispersion medium The composition containing these is mentioned.
  • a diffusion gas such as BBr 3 can be introduced into a heated diffusion furnace to diffuse and deposit the p-type donor element on the surface of the n-type semiconductor substrate.
  • the method for applying the boron-containing composition to the surface of the n-type semiconductor substrate is not particularly limited. Examples thereof include a printing method, a spin coating method, a brush coating, a spray method, a doctor blade method, a roll coating method, and an ink jet method.
  • a composition containing boron is applied to the n-type semiconductor substrate, and the p-type donor element can be diffused by heat treatment in a diffusion furnace.
  • the oxidation treatment is performed before the step of diffusing the p-type donor element, an oxide film functioning as a barrier layer is formed on the n-type diffusion layer before diffusing the p-type donor element. For this reason, even if the gas or composition containing a p-type donor element is used, it is easy to prevent the p-type donor element from diffusing into the n-type diffusion layer.
  • the method for manufacturing a solar cell element of the present invention includes a step of forming an electrode on a semiconductor substrate having an n-type diffusion layer manufactured by the method for manufacturing a semiconductor substrate having an n-type diffusion layer of the present invention.
  • the step of forming the electrode can be performed separately from the step of forming the n-type diffusion layer. Since it is possible to form the n-type diffusion layer and the electrode separately, as will be described later, there is a tendency for options such as the material of the electrode and the forming method to expand.
  • the material and forming method of the electrode are not particularly limited, and materials and forming methods known in the art can be adopted.
  • the material of the electrode is not limited to Group 13 aluminum used in the prior art, and Ag (silver), Cu (copper), etc. can be applied, and the thickness of the electrode is also thinner than the conventional one. It becomes possible to do.
  • a semiconductor substrate having an n-type diffusion layer manufactured by a method for manufacturing a semiconductor substrate having an n-type diffusion layer is manufactured using a specific n-type diffusion layer forming composition, it is selected as a desired portion of the semiconductor substrate. In particular, an n-type diffusion layer is formed.
  • a p-type diffusion layer is formed by applying a heat treatment by applying an aluminum paste as a group 13 element to an n-type diffusion layer formed in a region other than a desired region, and diffusing aluminum in the n-type diffusion layer.
  • the method of converting to is widely adopted. In this method, conversion to the p-type diffusion layer is sufficient, and in order to form a high-concentration electric field layer of the p + -type diffusion layer, a certain amount of aluminum is required. Need to form.
  • the thermal expansion coefficient of aluminum is significantly different from that of the semiconductor substrate, a large internal stress tends to be generated in the semiconductor substrate during the heat treatment and cooling. This internal stress damages the crystal grain boundary when crystalline silicon is used as the semiconductor substrate, and there is a problem that power loss increases in a solar cell using this semiconductor substrate.
  • the semiconductor substrate may be warped due to internal stress. The warpage of the semiconductor substrate facilitates damage of the solar cell element when transporting the solar cell element in the module process, connecting to a copper wire called a tab wire, or the like.
  • the silicon substrate which is a semiconductor substrate, has been thinned due to the improvement of the slicing technique, and the solar cell element is more easily damaged by warping.
  • a semiconductor substrate having an n-type diffusion layer in which an n-type diffusion layer is formed in a desired portion is used, other than the desired portion that has been performed by the conventional method.
  • Side etching or the like for removing the n-type diffusion layer formed on the substrate becomes unnecessary, and the process tends to be simplified.
  • the step of converting the n-type diffusion layer formed in a region other than the desired portion into the p + -type diffusion layer is not necessary, and the necessity of increasing the thickness of the aluminum layer is eliminated. As a result, generation of internal stress in the semiconductor substrate and warpage of the semiconductor substrate can be suppressed.
  • the method for forming the p + -type diffusion layer, the material, shape, thickness, etc. of the electrode are not limited to the conventional methods, and there are tendencies to expand the choices of manufacturing method, material, shape, etc. to be applied.
  • FIG. 1 is a schematic cross-sectional view conceptually showing an example of the manufacturing process of the solar cell element of the present invention.
  • symbol is attached
  • an alkaline solution is applied to a crystalline silicon substrate which is an n-type semiconductor substrate 1 to remove a damaged layer, and a texture structure is obtained by etching.
  • a texture structure is obtained by etching.
  • the damaged layer on the surface of the silicon substrate generated when slicing from the ingot is removed with 20% by mass caustic soda.
  • etching is performed using a mixed liquid of 1% by mass caustic soda and 10% by mass isopropyl alcohol to form a textured structure (in FIG. 1 (1), only one side of the n-type semiconductor substrate 1 has a description of the textured structure) To do).
  • the solar cell element by forming a texture structure on the light receiving surface (the lower surface in FIG. 1 (1)), a light confinement effect is promoted, and high efficiency is achieved.
  • the specific n-type diffusion layer forming composition according to the present invention is partially applied to the surface of the n-type semiconductor substrate 1, that is, the surface to be the light-receiving surface, thereby forming an n-type diffusion composition layer. 2 is formed.
  • the n-type semiconductor substrate 1 having the n-type diffusion composition layer 2 shown in FIG. 1 (2) is set to 600 ° C. to 1200 ° C., and the gas flow rate is set in the range of 3 mm / second to 60 mm / second in linear velocity.
  • Heat treatment thermal diffusion
  • the donor element diffuses into the semiconductor substrate, and the n-type diffusion layer 3 is formed.
  • a glass layer (not shown) such as phosphate glass is formed on the surface of the n-type diffusion layer 3.
  • the n-type semiconductor substrate 1 After the heat treatment, the n-type semiconductor substrate 1 is cooled to room temperature. Thereafter, the glass layer formed on the n-type semiconductor substrate 1 is removed by etching.
  • a silicon oxide film 4 shown in FIG. 1 (3) is formed by oxidation treatment.
  • the silicon oxide film 4 is formed thick in the region of the n-type diffusion layer 3 and thin in other regions.
  • the silicon oxide film 4 other than the region of the n-type diffusion layer 3 is removed by etching.
  • the thickness of the silicon oxide film formed in the region of the n-type diffusion layer 3 also tends to be reduced by etching. Therefore, the etching is stopped when the silicon oxide film 4 other than the region of the n-type diffusion layer 3 is sufficiently removed.
  • FIG. 1 (4) an n-type semiconductor substrate having the silicon oxide film 4 as a barrier layer only in the region of the n-type diffusion layer 3 is obtained.
  • a boron silicate glass layer 5 is formed on the n-type semiconductor substrate 1 and the silicon oxide film 4 shown in FIG. 1 (4), and a p-type diffusion layer 6 is formed by diffusing a p-type donor element.
  • a p-type diffusion layer 6 is formed in a region where the boron silicate glass layer 5 is in contact with the n-type semiconductor substrate 1.
  • the n-type diffusion layer 3 since the silicon oxide film 4 existing on the n-type diffusion layer 3 functions as a barrier layer, the donor element from the boron silicate glass layer 5 does not diffuse.
  • the boron silicate glass layer 5 and the silicon oxide film 4 are removed by etching to obtain the n-type semiconductor substrate 1 including the n-type diffusion layer 3 and the p-type diffusion layer 6 as shown in FIG.
  • the method for manufacturing the back contact type solar cell element including the n-type diffusion layer 3 and the p-type diffusion layer 6 on one surface of the n-type semiconductor substrate 1 has been described. However, if the method for producing a semiconductor substrate having an n-type diffusion layer of the present invention is used, a double-sided electrode type solar cell element can also be produced.
  • the method of manufacturing the back contact type solar cell element provided with the n-type diffusion layer and the p-type diffusion layer on one side of the n-type semiconductor substrate has been described.
  • An electrode-type solar cell element can also be manufactured.
  • Example 1 9. P 2 O 5 —SiO 2 —MgO glass (P 2 O 5 : 34%, SiO 2 : 39%, CaO: 27%) particles having an average particle size of 1 ⁇ m, 9 g of ethyl cellulose, 2.1 g of terpineol, and 18. 9 g was mixed to prepare a paste-like n-type diffusion layer forming composition. Next, the prepared n-type diffusion layer forming composition was applied to the surface of the n-type silicon substrate by screen printing and dried on a hot plate at 150 ° C. for 5 minutes. Next, it was kept in an oven set at 450 ° C. for 1.5 minutes to release ethyl cellulose.
  • the sheet resistance was measured at five points within the surface where the n-type diffusion layer forming composition of the obtained silicon substrate having a length of 156 mm and a width of 156 mm was applied. The standard deviation of the obtained sheet resistance was obtained, and the degree of variation in sheet resistance was evaluated based on the value calculated by dividing by the average value as a numerical value of 100 minutes.
  • the sheet resistance was measured by a four-probe method using a “Loresta-EP MCP-T360 type low resistivity meter” (Mitsubishi Chemical Corporation).
  • the silicon oxide film and the boron silicate glass film were removed by hydrofluoric acid etching.
  • the secondary ion mass spectrometer “IMS-7F” CAMECA
  • the n-type diffusion layer region of the obtained silicon substrate was subjected to a primary ion energy of 6000 eV while flowing oxygen gas into the analysis chamber. Secondary ion mass spectrometry was performed to a depth of 2 ⁇ m, and the amount of boron was measured. When the amount of boron was less than 1E16 (1 ⁇ 10 16 ) atoms / cm 3 , it was determined that the silicon oxide film had a barrier property. The results are shown in Table 1.
  • Example 2 to Example 4> Other than changing the linear velocity of the gas flowing in the diffusion furnace to 7 mm / second (Example 2), 10 mm / second (Example 3), or 20 mm / second (Example 4) during the thermal diffusion in Example 1 Performed the same treatment as in Example 1, and evaluated the average thickness of the silicon oxide film and the presence or absence of barrier properties. The results are shown in Table 1.

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Abstract

　La présente invention porte sur un procédé de fabrication de substrat semi-conducteur comprenant une couche de diffusion de type n comprenant une étape de traitement thermique d'un substrat semi-conducteur de telle sorte que le débit de gaz est de 3 à 60 mm/sec en vitesse linéaire, au moins une partie du substrat semi-conducteur étant en communication avec une composition de formation de couche de diffusion de type n qui contient un milieu de dispersion et des particules de verre contenant un élément donneur.
PCT/JP2015/070322 2014-07-15 2015-07-15 Procédé de fabrication de substrat semi-conducteur comprenant une couche de diffusion de type n, et procédé de fabrication d'élément de cellule solaire Ceased WO2016010095A1 (fr)

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JP2016534479A JPWO2016010095A1 (ja) 2014-07-15 2015-07-15 ｎ型拡散層を有する半導体基板の製造方法及び太陽電池素子の製造方法

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WO2013005738A1 (fr) * 2011-07-05 2013-01-10 日立化成工業株式会社 COMPOSITION POUR LA FORMATION D'UNE COUCHE DE DIFFUSION DE TYPE n, PROCÉDÉ POUR LA PRODUCTION D'UNE COUCHE DE DIFFUSION DE TYPE n ET PROCÉDÉ DE PRODUCTION D'ÉLÉMENTS DE CELLULE SOLAIRE
JP2013026467A (ja) * 2011-07-21 2013-02-04 Hitachi Chem Co Ltd ｎ型拡散層の製造方法、及び太陽電池素子の製造方法
JP2013026344A (ja) * 2011-07-19 2013-02-04 Hitachi Chem Co Ltd ｎ型拡散層の製造方法、太陽電池素子の製造方法、および太陽電池素子
JP2013026579A (ja) * 2011-07-25 2013-02-04 Hitachi Chem Co Ltd ｐ型拡散層の製造方法及び太陽電池素子の製造方法
JP2014086587A (ja) * 2012-10-24 2014-05-12 Sharp Corp 太陽電池セルの製造方法および太陽電池セル

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WO2013005738A1 (fr) * 2011-07-05 2013-01-10 日立化成工業株式会社 COMPOSITION POUR LA FORMATION D'UNE COUCHE DE DIFFUSION DE TYPE n, PROCÉDÉ POUR LA PRODUCTION D'UNE COUCHE DE DIFFUSION DE TYPE n ET PROCÉDÉ DE PRODUCTION D'ÉLÉMENTS DE CELLULE SOLAIRE
JP2013026344A (ja) * 2011-07-19 2013-02-04 Hitachi Chem Co Ltd ｎ型拡散層の製造方法、太陽電池素子の製造方法、および太陽電池素子
JP2013026467A (ja) * 2011-07-21 2013-02-04 Hitachi Chem Co Ltd ｎ型拡散層の製造方法、及び太陽電池素子の製造方法
JP2013026579A (ja) * 2011-07-25 2013-02-04 Hitachi Chem Co Ltd ｐ型拡散層の製造方法及び太陽電池素子の製造方法
JP2014086587A (ja) * 2012-10-24 2014-05-12 Sharp Corp 太陽電池セルの製造方法および太陽電池セル

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