CN118202443A - P-type impurity diffusion composition and method for manufacturing solar cell using same - Google Patents
P-type impurity diffusion composition and method for manufacturing solar cell using same Download PDFInfo
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- CN118202443A CN118202443A CN202280070587.6A CN202280070587A CN118202443A CN 118202443 A CN118202443 A CN 118202443A CN 202280070587 A CN202280070587 A CN 202280070587A CN 118202443 A CN118202443 A CN 118202443A
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- WRECIMRULFAWHA-UHFFFAOYSA-N trimethyl borate Chemical compound COB(OC)OC WRECIMRULFAWHA-UHFFFAOYSA-N 0.000 description 1
- DTBRTYHFHGNZFX-UHFFFAOYSA-N trioctyl borate Chemical compound CCCCCCCCOB(OCCCCCCCC)OCCCCCCCC DTBRTYHFHGNZFX-UHFFFAOYSA-N 0.000 description 1
- MDCWDBMBZLORER-UHFFFAOYSA-N triphenyl borate Chemical compound C=1C=CC=CC=1OB(OC=1C=CC=CC=1)OC1=CC=CC=C1 MDCWDBMBZLORER-UHFFFAOYSA-N 0.000 description 1
- LTEHWCSSIHAVOQ-UHFFFAOYSA-N tripropyl borate Chemical compound CCCOB(OCCC)OCCC LTEHWCSSIHAVOQ-UHFFFAOYSA-N 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 125000000391 vinyl group Chemical class [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
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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
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/18—Processes or apparatus specially adapted for the manufacture or treatment of these devices or of parts thereof
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- 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
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- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Electromagnetism (AREA)
- Photovoltaic Devices (AREA)
Abstract
The invention provides a p-type impurity diffusion composition which can achieve the thinning of patterns. A p-type impurity diffusion composition comprising (A) a group 13 element compound, (B) a hydroxyl group-containing polymer, and (C) an organic filler made of a polymer obtained by crosslinking.
Description
Technical Field
The present invention relates to a p-type impurity diffusion composition and a method for manufacturing a solar cell using the same.
Background
Conventionally, in the manufacture of solar cells, in the case of forming an n-type or p-type impurity diffusion layer in a semiconductor substrate, a method of forming a diffusion source on the substrate and diffusing impurities into the semiconductor substrate by thermal diffusion has been employed. The diffusion source may be formed by a CVD method or a solution coating method of the liquid impurity diffusion composition. For example, in the case of using the impurity diffusion composition in a liquid state, a thermal oxide film is first formed on the surface of a semiconductor substrate, and then a resist having a predetermined pattern is laminated on the thermal oxide film by photolithography. Then, the thermal oxide film portion not masked by the resist is etched with an acid or an alkali using the resist as a mask, and the resist is stripped to form a mask made of the thermal oxide film. Then, an n-type or p-type diffusion composition is applied to adhere the diffusion composition to the portions of the mask openings. Then, the impurity component in the composition is thermally diffused into the semiconductor substrate at 600 to 1250 ℃ to form an n-type or p-type impurity diffusion layer.
In recent years, it has been studied to manufacture a solar cell at low cost by simply performing fine patterning of an impurity diffusion layer region by a printing method or the like without using conventional photolithography techniques for manufacturing such a solar cell (for example, see patent document 1). Since the diffusion agent is selectively discharged directly to the doped layer formation region by a printing method without using a mask, a complicated process is not required and the amount of liquid used can be reduced as compared with the conventional photolithography method.
As a constituent component of an n-type or p-type impurity diffusion composition suitable for a printing system, it is known to use a polysiloxane (for example, see patent documents 2 to 5).
Prior art literature
Patent literature
Patent document 1: japanese patent application laid-open No. 2003-168810
Patent document 2: japanese patent laid-open No. 2002-539915
Patent document 3: japanese patent application laid-open No. 2012-114298
Patent document 4: japanese patent No. 6361505
Patent document 5: japanese patent application laid-open No. 2019-533026
Disclosure of Invention
Problems to be solved by the invention
However, with respect to these impurity diffusion compositions, the pattern becomes wide when printing and drying are performed, and it is difficult to form a fine line pattern. In general, thixotropic properties are imparted by the addition of a filler or the like to improve the composition, but in the case of a p-type impurity diffusion composition, it is considered that sufficient fine-line formation is not achieved due to poor dispersion of the filler or the like in the impurity diffusion composition.
The present invention has been made in view of the above circumstances, and an object thereof is to provide a p-type impurity diffusion composition capable of achieving fine line formation of a pattern.
Means for solving the problems
In order to solve the above problems, the p-type impurity diffusion composition of the present invention has the following constitution.
[1] A p-type impurity diffusion composition comprising (A) a group 13 element compound, (B) a hydroxyl group-containing polymer, and (C) an organic filler made of a polymer obtained by crosslinking.
[2] The p-type impurity diffusion composition according to [1], wherein the organic filler (C) made of a polymer obtained by crosslinking has an ethylene oxide or a propylene oxide.
[3] The p-type impurity diffusion composition according to [2], wherein the organic filler (C) made of a polymer obtained by crosslinking is a crosslinked body obtained by copolymerizing the following (C-1) compound with the (C-2) compound:
(C-1) a compound having at least 1 group selected from an acryl group and a methacryl group; and
(C-2) Compounds having an acryl group or a methacryl group bonded to both ends of a structure having an ethylene oxide or a propylene oxide.
[4] The p-type impurity diffusion composition according to any one of [1] to [3], wherein the hydroxyl group-containing polymer (B) is polyvinyl alcohol.
[5] The p-type impurity diffusion composition according to [4], wherein the saponification degree of the polyvinyl alcohol is 20 mol% or more and less than 70 mol%.
[6] The p-type impurity diffusion composition according to any one of [1] to [5], which contains 1, 3-propanediol as a solvent.
[7] A method for manufacturing a solar cell includes a step of forming an impurity diffusion layer at 2 or more levels of different impurity concentrations,
The forming of the impurity diffusion layer of at least 1 level or more includes the steps of:
A step of partially forming an impurity diffusion composition film (a) by applying the p-type impurity diffusion composition of any one of [1] to [6] to a semiconductor substrate; and
And (b) heating the obtained impurity diffusion composition film (a) to diffuse the impurities into the semiconductor substrate and form an impurity diffusion layer (b).
[8] The method for manufacturing a solar cell according to [7], comprising a step of diffusing an impurity into a portion where the impurity diffusion composition film (a) is not formed, using the impurity diffusion composition film (a) as a mask.
[9] The method of manufacturing a solar cell according to [8], wherein the step of diffusing the impurity into the portion where the impurity diffusion composition film (a) is not formed is a step of heating in an atmosphere containing an impurity diffusion component.
Effects of the invention
According to the present invention, a p-type impurity diffusion composition capable of achieving fine patterning can be provided.
Drawings
Fig. 1 is a process cross-sectional view showing an example of a method for producing a solar cell using the p-type impurity diffusion composition of the present invention.
Detailed Description
Hereinafter, preferred embodiments of the p-type impurity diffusion composition and the method for manufacturing a semiconductor element using the same according to the present invention will be described in detail with reference to the drawings as necessary. The present invention is not limited to these embodiments.
The p-type impurity diffusion composition of the present invention comprises (A) a group 13 element compound, (B) a hydroxyl group-containing polymer, and (C) an organic filler made of a polymer obtained by crosslinking.
((A) group 13 element Compound)
The p-type impurity diffusion composition of the present invention contains a group 13 element compound as an impurity diffusion component, whereby a p-type impurity diffusion layer can be formed in a semiconductor substrate. The group 13 element compound is preferably a boron compound.
Examples of the boron compound include boric acid, diboron trioxide, methyl boric acid, phenyl boric acid, trimethyl borate, triethyl borate, tripropyl borate, tributyl borate, trioctyl borate, and triphenyl borate. Among them, boric acid and diboron trioxide are preferable from the viewpoint of doping.
The content of the group 13 element compound (a) contained in the p-type impurity diffusion composition may be arbitrarily determined depending on the resistance value required for the semiconductor substrate, but is preferably 0.1 to 10 mass%, more preferably 0.5 to 5 mass%, of 100 mass% of the entire composition.
((B) Polymer containing hydroxyl group)
In the p-type impurity diffusion composition of the present invention, the hydroxyl group-containing polymer (B) is a component for forming a complex with the group 13 element compound (a) (particularly preferably, a boron compound) and forming a uniform coating film at the time of coating.
The hydroxyl group-containing polymer (B) includes, specifically, polyvinyl alcohol resins such as polyvinyl alcohol and modified polyvinyl alcohol, polyvinyl alcohol derivatives such as polyvinyl acetal and polyvinyl butyral, polyoxyalkylene groups such as polyoxyethylene and polyoxypropylene, and polyhydroxyacrylates such as hydroxyethyl cellulose, polymethyl acrylate, hydroxyethyl polyacrylate and hydroxypropyl polyacrylate. Among them, polyvinyl alcohol is preferable in terms of the formability of a complex with (a) a group 13 element compound (particularly preferably a boron compound), the stability of the formed complex, and the storage stability of the p-type impurity diffusion composition.
From the viewpoint of complex stability, the saponification degree of polyvinyl alcohol is preferably 20 mol% or more and less than 70 mol%. By setting the saponification degree to 20% or more, the stability of the complex formed with the impurity diffusion component (a) is improved, and low resistance, improved uniformity of resistance, and improved carrier lifetime can be expected. Further, the saponification degree is less than 70%, whereby (C) the dispersibility of the organic filler made of the crosslinked polymer is improved, and the low resistance value, the resistance uniformity and the carrier lifetime can be expected to be improved. The saponification degree of polyvinyl alcohol is more preferably 30 mol% or more and less than 50 mol% from the viewpoint of improvement of storage stability. The average degree of polymerization of the polyvinyl alcohol is most preferably 150 to 1000 in terms of solubility and stability of the complex. In the present invention, the average polymerization degree and the saponification degree are both values measured in accordance with JIS K6726 (1994). The saponification degree is a value measured by the back titration method in the method described in the JIS.
The content of the hydroxyl group-containing polymer (B) is preferably 1 to 20 mass%, more preferably 5 to 15 mass% based on 100 mass% of the entire composition, from the viewpoints of good heat diffusion and suppression of organic residues on the substrate after removal of the composition.
From the viewpoint of uniformity of diffusion, the mass ratio (A) of the group 13 element compound (A) to the hydroxyl group-containing polymer (B) is preferably 1:20 to 1:1, more preferably 1:15 to 1:3.
((C) organic filler made of crosslinked polymer)
In order to impart thixotropic properties and achieve improvement in printing characteristics, it is important that the p-type impurity diffusion composition of the present invention contains (C) an organic filler made of a polymer that is crosslinked. The thixotropic property is a ratio (η 1/η2) of the viscosity (η 1) at the time of increasing the low shear stress to the viscosity (η 2) at the time of increasing the high shear stress. By making the thixotropic property large, the pattern accuracy of screen printing can be improved. This is due to the reasons described below. The p-type impurity diffusion composition having high thixotropic properties has a low viscosity at high shear stress, and thus is less likely to cause clogging of a screen at screen printing, and has a high viscosity at low shear stress, and thus is less likely to cause bleeding immediately after printing and thickening of pattern line width.
The thixotropic property can be obtained from the ratio of the viscosities at different rotational speeds obtained by the above-described viscosity measurement method. In the present invention, the ratio (. Eta. 2/η20) of the viscosity (. Eta. 20) at 20rpm to the viscosity (. Eta. 2) at 2rpm is defined as thixotropic property. In order to form a pattern with good precision by screen printing, the thixotropic property is preferably 2 or more, and more preferably 3 or more.
In addition, (C) the organic filler made of the crosslinked polymer has the following effects: the complex of the group 13 element compound (A) and the hydroxyl group-containing polymer (B) is stabilized, and dispersibility in these complexes is improved, thereby contributing to thinning of the pattern, further improving uniformity of the resistance value after diffusion, reducing the resistance value, and improving carrier lifetime.
Specific examples of the crosslinked polymer include, but are not limited to, polymers of acryl compounds, methacryl compounds, vinyl compounds, epoxy compounds, and phenol compounds.
The organic filler (C) made of a polymer obtained by crosslinking preferably has ethylene oxide or propylene oxide from the viewpoints of further stabilizing the complex and improving uniformity of resistance after diffusion and reduction of residue after removal of the composition film. The ethylene oxide or propylene oxide may be contained in the network of the network structure of the crosslinked polymer, or may be contained at the terminal of the network structure.
(C) The organic filler made of the crosslinked polymer is more preferably a crosslinked product obtained by copolymerizing (C-1) a compound having at least 1 group selected from among an acryl group and a methacryl group and (C-2) a compound having an oxyethylene group or oxypropylene group bonded to both ends of the structure. Thus, in addition to the ethylene oxide or propylene oxide of (C-2), the carbonyl group in the acryl or methacryl group of (C-1) contributes to further stabilization of the complex formed by the group 13 element compound of (A) and the hydroxyl group-containing polymer of (B). As a result, it is expected that the pattern will be thinner, the resistance will be lower, the uniformity of the resistance will be higher, and the carrier lifetime will be longer.
Specific examples of the compound (C-1) having at least 1 group selected from the group consisting of an acryl group and a methacryl group include, but are not limited to, acrylic acid, methacrylic acid, methyl acrylate, methyl methacrylate, 2-hydroxyethyl acrylate, 2-hydroxyethyl methacrylate, glycidyl acrylate, glycidyl methacrylate, and the like.
Specific examples of the compound (C-2) having an acryl or methacryl group bonded to both ends of the structure having an ethylene oxide or propylene oxide include, but are not limited to, polyethylene glycol diacrylate, polyethylene glycol dimethacrylate, ethylene glycol diacrylate, ethylene glycol dimethacrylate, diethylene glycol diacrylate, diethylene glycol dimethacrylate, dipropylene glycol diacrylate, dipropylene glycol dimethacrylate, polypropylene glycol diacrylate, polypropylene glycol dimethacrylate, and the like.
From the viewpoint of further stabilizing the complex of the group 13 element compound (A) and the hydroxyl group-containing polymer (B), the amount of (C-2) is preferably 0.5 to 20 mol%, more preferably 1 to 10 mol%, relative to 100 mol% of (C-1).
These compounds may be obtained by polymerizing a radical polymerization initiator such as azobisisobutyronitrile in a good solvent at 60 to 100 ℃, separating the resulting crosslinked product by a method such as filtration, and pulverizing the crosslinked product to obtain fine particles, thereby obtaining (C) an organic filler made of a crosslinked polymer. Or suspension polymerization in a poor solvent at 60 to 100℃and separation of the resulting fine particles.
When the hydroxyl group-containing polymer (B) is 100 mass%, the p-type impurity diffusion composition of the present invention preferably contains 100 to 1000 mass% of (C) an organic filler made of a crosslinked polymer. Preferably 200 to 700 mass%.
(Solvent)
The p-type impurity diffusion composition of the present invention preferably further comprises a solvent. The solvent herein means a solvent which is liquid at normal pressure and at 23 ℃ and which can dissolve the hydroxyl group-containing polymer (B) and disperse the organic filler (C) made of the crosslinked polymer. The content of the solvent is preferably 10 to 90% by mass, more preferably 20 to 70% by mass, based on 100% by mass of the entire composition.
The solvent may be used without particular limitation, but from the viewpoint of further improving printability by screen printing, spin-coating printing, or the like, a solvent having a boiling point of 100 ℃ or higher is preferred. When the boiling point is 100 ℃ or higher, for example, when the p-type impurity diffusion composition is printed on a printing plate used in the screen printing method, drying and adhesion of the p-type impurity diffusion composition on the printing plate can be suppressed. Preferably 160℃or higher, more preferably 180℃or higher.
The content of the solvent having a boiling point of 100 ℃ or higher is preferably 20% by weight or higher relative to the total amount of the solvent. Examples of the solvent having a boiling point of 100℃or higher include ethyl lactate (boiling point 155 ℃), diacetone alcohol (boiling point 169 ℃), propylene glycol monomethyl ether acetate (boiling point 145 ℃), propylene glycol monomethyl ether (boiling point 120 ℃), 3-methoxy-3-methyl-1-butanol (boiling point 174 ℃), gamma-butyrolactone (boiling point 204 ℃), N-methyl-2-pyrrolidone (boiling point 204 ℃), N-dimethylimidazolidinone (boiling point 226 ℃), terpineol (boiling point 219 ℃) and 1, 3-propanediol (214 ℃).
In addition, the solvent more preferably contains 1, 3-propanediol. By containing 1, 3-propanediol, the stability of the complex formed by the group 13 element compound (A) and the hydroxyl group-containing polymer (B) is further improved. As a result, the formation of a three-dimensional complex by further reacting the group 13 element compound (a) having formed a complex with the hydroxyl group-containing polymer (B) is easily suppressed, and thickening of the p-type impurity diffusion composition with time and the generation of gel-like foreign matter due to thickening are easily suppressed. This improves the uniformity of the resistance value and makes the pattern thinner, and even when the p-type impurity diffusion composition is left at room temperature, the uniformity of the resistance value is not impaired, and the p-type impurity diffusion composition can be used stably.
(Thixotropic agent)
The p-type impurity diffusion composition of the present invention may contain a thixotropic agent in addition to (C) the organic filler made of the crosslinked polymer, in a range where the fine line of the pattern is not impaired and the influence of the residual inorganic component does not exist, in terms of improvement of printability.
Specifically, cellulose derivatives, sodium alginate, polysaccharides, bentonite, montmorillonite, fine particles of silicon oxide (fine particle silicon oxide), colloidal alumina, calcium carbonate, and the like can be exemplified. The fine particles of silicon oxide are preferable in terms of compatibility with other components in the composition and reduction of residue.
The viscosity of the p-type impurity diffusion composition of the present invention is not limited, and may be appropriately changed according to the printing method and the film thickness. Here, for example, in the case of a screen printing method which is one of preferred printing methods, the viscosity of the diffusion composition is preferably 5,000mpa·s or more. This is because bleeding of the printed pattern can be suppressed to obtain a good pattern. Further preferably, the viscosity is 10,000 mPas or more. The upper limit is not particularly limited, but is preferably 100,000mpa·s or less from the viewpoints of storage stability and handleability.
Here, the viscosity is a value measured at 20rpm using a type E digital viscometer based on JIS Z8803 (1991) "solution viscosity-measuring method", and the viscosity is a value measured at 20rpm using a type B digital viscometer based on JIS Z8803 (1991) "solution viscosity-measuring method", when the viscosity is 1,000mpa·s or more.
(Surfactant)
The p-type impurity diffusion composition of the present invention may contain a surfactant. By containing the surfactant, coating unevenness is improved, and a more uniform coating film can be obtained. As the surfactant, a fluorine-based surfactant and a silicone-based surfactant are preferably used. When the surfactant is contained, the content of the surfactant is preferably set to 0.0001 to 1% by weight in the p-type impurity diffusion composition.
(Concentration of solid component)
In the p-type impurity diffusion composition of the present invention, the solid content concentration is not particularly limited, but the preferable range is 1 mass% or more and 90 mass% or less. If the concentration is less than this range, the coating film thickness becomes too thin, and it may be difficult to obtain desired doping and masking properties. If the concentration is higher than this range, the storage stability may be lowered.
The p-type impurity diffusion composition of the present invention can be used for photovoltaic elements such as solar cells, semiconductor devices in which an impurity diffusion region is patterned on the surface of a semiconductor, for example, transistor arrays, diode arrays, photodiode arrays, converters, and the like.
< Method for producing solar cell >
The method for manufacturing a solar cell of the present invention is a method for manufacturing a solar cell including a step of forming an impurity diffusion layer at 2 or more levels of different impurity concentrations,
The forming of the impurity diffusion layer of at least 1 level or more includes the steps of:
a step of partially forming an impurity diffusion composition film (a) by applying the p-type impurity diffusion composition of the present invention to a semiconductor substrate; and
And (b) heating the obtained impurity diffusion composition film (a) to diffuse the impurities into the semiconductor substrate and form an impurity diffusion layer (b).
The different impurity concentrations herein mean that the difference in impurity concentration is 1×10 17atoms/cm3 or more, and the difference in sheet resistance value of the substrate surface at the portion where the impurity diffusion layer is formed is 10Ω/≡or more. The present embodiment will be described in detail below.
First, as shown in fig. 1 (i), the p-type impurity diffusion composition of the present invention is partially applied to a semiconductor substrate 1 to form a pattern 2 of a p-type impurity diffusion composition film (a).
Examples of the semiconductor substrate include n-type single crystal silicon and polycrystalline silicon having an impurity concentration of 10 15～1016atoms/cm3, and a crystalline silicon substrate mixed with other elements such as germanium and carbon. P-type single crystal silicon, semiconductors other than silicon may also be used.
The semiconductor substrate preferably has a thickness of 50 to 300 μm and an outline of a substantially quadrangular shape having one side of 100 to 250 mm. In order to remove the dicing damage and the natural oxide film, the semiconductor substrate surface is preferably etched in advance with a hydrofluoric acid solution, an alkali solution, or the like. At this time, innumerable uneven textures having a typical width of 40 to 100 μm and a depth of 3 to 4 μm are formed on the surface of the semiconductor substrate.
Regarding the process of forming the impurity diffusion layer at 2 or more levels of different impurity concentrations, the formation of at least 1 or more levels of impurity diffusion layers includes the following processes: a step of partially forming a p-type impurity diffusion composition film (a) by applying the p-type impurity diffusion composition of the present invention to a semiconductor substrate; and a step of heating the substrate to diffuse the impurities into the semiconductor substrate to form an impurity diffusion layer (b).
Examples of the method for applying the p-type impurity diffusion composition include spin coating, screen printing, inkjet printing, slit coating, spray coating, relief printing, and gravure printing.
Preferably, after the p-type impurity diffusion composition is applied by these methods, the semiconductor substrate 1 coated with the p-type impurity diffusion composition is dried at 50 to 300 ℃ for 30 seconds to 30 minutes by using a heating plate, an oven, or the like, thereby desolvation is performed to form the pattern 2 of the p-type impurity diffusion composition film (a).
The film thickness of the dried p-type impurity diffusion composition film (a) is preferably 100nm or more from the viewpoint of the diffusivity of impurities, and preferably 7 μm or less from the viewpoint of the residue after etching.
Next, as shown in fig. 1 (ii), the impurity diffusion composition film (a) is heated to be diffused into the semiconductor substrate 1, thereby forming an impurity diffusion layer (b). The method for diffusing the impurities may be a known thermal diffusion method, and may be, for example, electric heating, infrared heating, laser heating, microwave heating, or the like.
The time and temperature of thermal diffusion can be appropriately set so as to obtain desired diffusion characteristics such as impurity concentration and diffusion depth. For example, a diffusion layer having a surface impurity concentration of 10 19～1021atoms/cm3 can be formed by heating and diffusing at 800 ℃ or higher and 1200 ℃ or lower for 1 to 120 minutes.
The diffusion atmosphere is not particularly limited, and may be performed in the atmosphere, or an inert gas such as nitrogen or argon may be used to appropriately control the amount of oxygen in the atmosphere. From the viewpoint of shortening the diffusion time, the oxygen concentration in the atmosphere is preferably 3% or less. If necessary, the p-type impurity diffusion composition film (a) may be calcined at a temperature in the range of 200 to 850 ℃ before diffusion to decompose and remove the organic substances.
The step of forming an impurity diffusion layer at 2 or more levels of different impurity concentrations using the p-type impurity diffusion composition of the present invention preferably includes a step of diffusing an impurity into a portion where the impurity diffusion composition film (a) is not formed, using the impurity diffusion composition film (a) as a mask. Specifically, as shown in fig. 1 (iii), an impurity diffusion layer (c) having conductivity similar to that of the impurity diffusion layer (b) and having a different impurity concentration is formed on the unpatterned portion using the pattern 2 of the impurity diffusion composition film (a) as a mask.
The step of diffusing the impurity into the portion where the impurity diffusion composition film (a) is not formed (the step of forming the impurity diffusion layer (c)) using the impurity diffusion composition film (a) as a mask may be performed after the impurity diffusion composition film (a) is heated to diffuse the impurity into the semiconductor substrate 1 to form the impurity diffusion layer (b).
Specific examples of the method for diffusing the impurities into the portion where the impurity diffusion composition film (a) is not formed include the following methods: a method of implanting ions containing an impurity diffusion component into the semiconductor substrate 1 having the pattern 2 of the impurity diffusion composition film (a) and then annealing; a method of heating the semiconductor substrate 1 having the pattern 2 of the impurity diffusion composition film (a) in an atmosphere containing an impurity diffusion component; a method in which an impurity diffusion composition having conductivity similar to that of the semiconductor substrate 1 having the pattern 2 of the impurity diffusion composition film (a) and having a different impurity concentration is applied to a portion where the impurity diffusion composition film (a) is not formed, and after forming the impurity diffusion composition film, electric heating, infrared heating, laser heating, microwave heating, and the like are performed.
Among them, the step of diffusing the impurity to the portion where the impurity diffusion composition film (a) is not formed is preferably a step of heating in an atmosphere containing an impurity diffusion component.
When heating in an atmosphere containing an impurity diffusion component, for example, boron bromide (BBr 3) is bubbled in the p-type, phosphorus oxychloride (POCl 3) is bubbled in the N-type, and while the atmosphere containing an impurity diffusion component is produced by flowing through N 2, the semiconductor substrate 1 with the pattern 2 of the impurity diffusion composition film (a) is heated at 800 to 1000 ℃. By setting the gas pressure and the heating conditions, the impurity concentration of the impurity diffusion layer (c) can be set higher than the impurity concentration of the impurity diffusion layer (b), or the impurity concentration of the impurity diffusion layer (c) can be set lower than the impurity concentration of the impurity diffusion layer (b).
As shown in fig. 1 (i), after pattern 2 of the impurity diffusion composition film (a) is formed by partially applying the p-type impurity diffusion composition of the present invention to the semiconductor substrate 1, the pattern may be put into a heating furnace of fig. 1 (iii) without performing the diffusion step of fig. 1 (ii), and the impurity diffusion layer (b) and the impurity diffusion layer (c) may be simultaneously formed by heating in an atmosphere containing an impurity diffusion component.
As shown in fig. 1 (i), after pattern 2 of the impurity diffusion composition film (a) is formed by partially applying the p-type impurity diffusion composition of the present invention to the semiconductor substrate 1, the film may be put into a heating furnace of fig. 1 (iii) without performing the diffusion step of fig. 1 (ii), and first, the film may be heated only in an inert gas to form an impurity diffusion layer (b), and in this state, a gas containing an impurity diffusion component may be additionally introduced into the furnace, and the film may be heated under a condition different from that of the film when only the inert gas is used, thereby forming an impurity diffusion layer (c) having an impurity concentration different from that of the impurity diffusion layer (b) in one batch.
In the step (iii) of fig. 1, the surface of the semiconductor substrate where the impurity diffusion composition film (a) is not formed is oxidized to form a layer (d) containing silicon oxide such as borosilicate glass when the impurity is p-type, and to form a layer (d) containing silicon oxide such as phosphosilicate glass when the impurity is n-type.
< Etching Process >
After the step of forming the impurity diffusion layer at 2 or more levels of different impurity concentrations in this way, it is preferable to remove the pattern 2 of the impurity diffusion composition film (a) and the layer (d) containing silicon oxide formed on the surface as shown in fig. 1 (iv).
The pattern 2 of the impurity diffusion composition film (a) and the layer (d) containing silicon oxide can be removed by a known etching method. The material used for etching is not particularly limited, and for example, a material containing at least 1 of hydrogen fluoride, ammonium, phosphoric acid, sulfuric acid, and nitric acid as an etching component and containing water, an organic solvent, and the like as other components is preferable.
< Back surface Forming Process >
The method for manufacturing a solar cell according to the present invention may include a back surface forming step.
For example, in the case where a p-type impurity diffusion layer is formed on the surface of a substrate at 2 or more levels of different impurity concentrations and an n-type impurity diffusion layer is formed on the back surface, the surface is protected by a SiO 2 film or the like so that n-type impurities do not spread to the surface. The preferable film thickness for obtaining the protective effect is 100 to 1000nm, and it is preferable to form the film by plasma CVD having a high film formation rate at a low temperature in order to suppress the influence of the substrate surface on the p-type diffusion layer. More specifically, the film is formed under the conditions that the flow rate ratio of the mixed gas SiH 4/N2 O is 0.01-5.0, the pressure of the reaction chamber is 0.1-4 Torr, and the temperature during film forming is 300-550 ℃.
Then, phosphorus oxychloride (POCl 3) was bubbled through the back surface, and the semiconductor substrate was heated at 800 to 900 ℃ while an atmosphere containing an impurity diffusion component was produced by flowing through N 2. At this time, an n-type impurity diffusion layer is formed on the back surface of the substrate, and a layer containing silicon oxide such as a phosphosilicate glass layer is formed on the outermost portion of the back surface by oxidation.
Further, the inorganic film on the front surface and the layer containing silicon oxide on the back surface of the substrate are removed by etching. The specific example of the preferable etching is the same as the specific example when the impurity diffusion layer is formed at 2 or more levels of different impurity concentrations.
< Passivation Process >
In the method for manufacturing a solar cell of the present invention, when the back surface forming step is provided after the etching step, it is preferable that passivation films for suppressing recombination of the surfaces and preventing reflection of light are provided on the front and back surfaces of the semiconductor substrate thereafter. For example, siO 2 obtained by heat treatment in an oxygen atmosphere at a high temperature of 700 ℃ or higher as a passivation film of the p-type diffusion layer, and a silicon nitride film for protecting the film may be provided. In addition, only the SiN x film may be formed. In this case, the material may be formed by a plasma CVD method using a mixed gas of SiH 4 and NH 3 as a raw material. At this time, hydrogen diffuses into the crystal, and defects are passivated (hydrogen passivation) by orbitals that do not contribute to the bonding of silicon atoms, i.e., dangling bonds and hydrogen bonding. More specifically, the reaction mixture is formed under the conditions that the flow rate ratio NH 3/SiH4 is 0.05-5.0, the pressure of the reaction chamber is 0.1-4 Torr, and the temperature during film forming is 300-550 ℃.
< Electrode Forming Process >
Next, a metal paste was printed by screen printing so as to reach the high concentration impurity diffusion layer out of the 2 horizontal impurity diffusion layers from above the passivation film, and dried to form an electrode. The metal paste for an electrode contains metal particles and glass particles as essential components, and if necessary, a resin binder, other additives, and the like. The metal particles used in this case are preferably Ag or Al.
< Electrode firing Process >
Then, the electrode is heat-treated (fired) to complete the solar cell. When heat treatment (firing) is performed in a range of 600 to 900 ℃ for several seconds to several minutes, the antireflection film as an insulating film is melted by glass particles contained in the electrode metal paste on the light receiving surface side, and further, a part of the silicon surface is melted, and metal particles (for example, silver particles) in the paste form contact portions with the semiconductor substrate and solidify. The light-receiving surface electrode thus formed is electrically connected to the semiconductor substrate. This is called fire-through.
The light-receiving surface electrode is generally constituted by a bus bar electrode and finger electrodes intersecting the bus bar electrode. Such a light-receiving surface electrode can be formed by means of screen printing of the above-mentioned metal paste, plating of an electrode material, vapor deposition of an electrode material by electron beam heating in a high vacuum, or the like. The bus bar electrode and the finger electrode may be formed by a known method.
The method of manufacturing a solar cell according to the present invention is not limited to the above-described embodiment, and various modifications such as design changes may be applied based on the knowledge of those skilled in the art, and embodiments to which such modifications are applied are also included in the scope of the present invention.
Examples
The present invention will be described more specifically with reference to the following examples, but the present invention is not limited to these examples.
(1) Evaluation of residue on substrate
As a substrate, a semiconductor substrate (silicon wafer) made of n-type single crystal silicon having one side of 156mm was prepared, and both surfaces were alkali etched to remove slicing damage and native oxide. At this time, innumerable irregularities (textures) having a typical width of 40 to 100 μm and a depth of about 3 to 4 μm are formed on both surfaces of the semiconductor substrate, and this is used as a coated substrate.
A screen printer (model TM-750) was used, and a screen mask (manufactured by SUS (strain), 400 mesh, wire diameter 23 μm) having openings of the same size as the substrate was used as a screen mask, to screen-print the entire surface of the substrate.
After the p-type impurity diffusion compositions 1 to 9 were screen-printed, the substrate was heated in air at 200℃for 10 minutes, thereby forming an impurity diffusion composition film having a thickness of about 3.5. Mu.m.
Next, each substrate was placed in an electric furnace, and the impurity was thermally diffused by maintaining the substrate at 950 ℃ for 60 minutes in an atmosphere of nitrogen: oxygen=99:1 (volume ratio).
Each substrate after thermal diffusion was immersed in a 5 wt% aqueous hydrofluoric acid solution at 23 ℃ for 1 minute, and the impurity diffusion composition film was removed. After removal, the substrate was immersed in pure water and washed, and the presence or absence of residues was observed by visual observation of the surface. The surface deposit was visually confirmed after 1 minute of immersion, but the surface deposit was removed by rubbing with a wiper, the surface deposit was visually confirmed within more than 30 seconds and 1 minute was evaluated as B, the surface deposit was visually confirmed within 30 seconds was evaluated as a, and B or more were considered as acceptable.
(2) Resistance value evaluation
The substrate on which the impurities used for residue evaluation were diffused was subjected to p/n determination using a p/n determiner, and the surface resistance was measured using a four-probe type surface resistance measuring device RT-70V (manufactured by nalsocket). The measurement was performed on data of 13 points in total at intervals of 20mm in the vertical/horizontal direction from the center of the square substrate, and the average value was used as a sheet resistance value, and the variation in value was used as uniformity of the resistance value. The sheet resistance value is an index of the diffusivity of the impurity, and a smaller value means a larger diffusion amount of the impurity. The smaller the value, the better the deviation of the value indicating the uniformity of the resistance value, and the more up and down to 20% of the average value will be considered as acceptable.
(3) Screen printability (minimum pattern evaluation)
The p-type impurity diffusion compositions of each example and comparative example were patterned in a striped pattern by screen printing, and the stripe width accuracy was confirmed.
The same substrate as the coated substrate used for residue evaluation was used as the coated substrate.
A screen printer similar to the screen printer used for residue evaluation was used, and a screen mask (manufactured by SUS (strain), 400 mesh, wire diameter 23 μm) having 7 stripe-shaped parallel patterns was used as the screen mask, wherein a total of 7 openings (1 on the center line of the substrate (parallel to the side of the substrate) and 3 on the two outer sides of the substrate) having a width of 70 μm and a length of 13.5cm were formed in parallel with each other with the opening sandwiched therebetween.
After the p-type impurity diffusion compositions 1 to 9 were screen-printed, the substrate was heated in air at 200 ℃ for 10 minutes, thereby forming a pattern having a thickness of about 3.5 μm.
At this time, the width of the pattern printed with a 70 μm mask was measured using a microscope (MX 61L-zen), and the degree of widening of the pattern with respect to the 70 μm mask was evaluated, and 150 μm or less was regarded as acceptable.
(4) Carrier lifetime determination
The substrate used for evaluation of uniformity of the resistance was set at Photoconductance LIFETIME TESTER (WCT-120 SINTON CONSULTING INC. Manufactured) and the open circuit voltage Voc (Voltage Open Circuit) was measured. The higher Voc is, the longer the carrier lifetime is, the better the characteristics of the solar cell.
(5) Evaluation of stability over time
The p-type impurity diffusion compositions 1 to 9 were left at 25℃for 14 days, and after leaving for standing, the uniformity of the resistance value of (2) was evaluated. In this case, the variation in the value indicating the uniformity of the resistance value was considered to be acceptable within 20% of the average value.
Synthesis example 1
Synthesis of organic filler A made of crosslinked Polymer
21.3G of 2-hydroxyethyl acrylate (manufactured by Tokyo chemical industry Co., ltd.), 0.1g of polyethylene glycol diacrylate (A-400 manufactured by Xinzhongcun chemical industry Co., ltd.) and 59.1g of pure water were charged into a 250ml polypropylene container. Next, stirring was started by a magnetic stirrer, and nitrogen substitution was performed at 100 ml/min for 30 minutes. Then, the temperature was raised to 50℃while continuing stirring. After the liquid temperature was stabilized at 50 ℃, 0.6g of a 10 mass% aqueous solution of 2,2' -azobis (2-methylpropionamidine) dihydrochloride (manufactured by tokyo chemical industry Co., ltd.) was added as an initiator to initiate polymerization. After the polymerization reaction was carried out to form a gel, the gel was cured at 90℃for 30 minutes to terminate the polymerization. The obtained gel was pulverized and dried at 120℃for 2 hours, whereby an organic filler A having an average particle diameter of about 3 μm was obtained.
Synthesis example 2
Synthesis of organic filler B made of crosslinked Polymer
A commercially available bisphenol a diglycidyl ether type epoxy resin (jER 828: to a three-necked flask of 10.0g to 100cc, manufactured by millipore d polyethylene, and having an epoxy equivalent of 186), a surfactant (of which the surface active agent (of the co-polymer, EA-137) was added: 0.8g of the first Industrial pharmaceutical Co., ltd.) was kneaded for 1 minute. Then, 6cc of water contained in the syringe was added sequentially with stirring at 1.5cc intervals of 1 minute. A milky white emulsion was obtained in the flask.
To this uncured epoxy emulsion was added a curing liquid obtained by dissolving 0.6 equivalent of piperazine in 8cc of water, and the mixture was homogenized by stirring slowly. The liquid was allowed to stand at 25℃for 3 days to solidify it into a spherical filler having an average particle diameter of about 6. Mu.m.
The above-mentioned filtered filler was charged into an eggplant-shaped flask, and 400g of acetonitrile (manufactured by tokyo chemical industry Co., ltd.) was added thereto to redisperse. The condenser was mounted thereon, and extraction was performed under heating and stirring in a water bath at 50℃for 8 hours, whereby the filler was purified. After cooling, suction filtration was performed, and drying was performed under reduced pressure at 50℃for 8 hours to obtain an organic filler B.
Synthesis example 3
Synthesis of organic filler C made of crosslinked Polymer
An organic filler C was obtained in the same manner as in Synthesis example 2 except that 10.0g of jER828 (manufactured by Abelmoschus, inc. of epoxy equivalent 186) was used instead of 10.0g of bisphenol A diglycidyl ether type epoxy resin (manufactured by Abelmoschus, inc.), and 2.0g of jER8288.0g of diethylene glycol diglycidyl ether (manufactured by Abelmoschus 100E: manufactured by Emblica chemical Co., ltd.) was added.
Synthesis example 4
< Synthesis of organic filler D made of uncrosslinked Polymer >
To the separable flask, 1.5g of polyvinylidene fluoride (manufactured by the chemical industry Co., ltd.), 7.5g of hydroxypropyl cellulose (manufactured by the chemical industry Co., ltd.), and 41.0g of acetone (manufactured by the chemical industry Co., ltd.) were charged, and stirring was performed at 50 ℃. The interior becomes cloudy and forms an emulsion. Then, 100g of water was added at a rate of 0.41 g/min, and after the entire amount of water was charged, the temperature was lowered to room temperature with stirring, the resulting suspension was filtered, washed with 100g of ion-exchanged water, and the resultant was separated by filtration and dried under vacuum at 80℃for 10 hours to obtain spherical organic filler D having a particle size of about 6. Mu.m.
Example 1
1.5G of boric acid (Fuji-F) and polyvinyl alcohol (PVA (80) manufactured by Nippon Corp.) having a saponification degree of 80% (hereinafter referred to as "PVA (80)) were mixed and stirred sufficiently to be uniform, and 34.0g of 3-methoxy-3-methyl-1-butanol (manufactured by Tokyo chemical Co., ltd.) (hereinafter referred to as" MMB ") and 20.0g of water were mixed to obtain a p-type impurity diffusion composition 1.
Example 2
A p-type impurity diffusion composition 2 was obtained in the same manner as in example 1, except that the organic filler B was used instead of the organic filler a.
Example 3
A p-type impurity diffusion composition 3 was obtained in the same manner as in example 1, except that the organic filler C was used instead of the organic filler a.
Comparative example 1
A p-type impurity diffusion composition 4 was obtained in the same manner as in example 1, except that the organic filler D was used instead of the organic filler a.
Comparative example 2
A p-type impurity diffusion composition 5 was obtained in the same manner as in example 1, except that a silica filler (SO-E2: mass) was used instead of the organic filler a.
Comparative example 3
A p-type impurity diffusion composition 6 was obtained in the same manner as in example 1, except that the organic filler a was not used.
Example 4
A p-type impurity diffusion composition 7 was obtained in the same manner as in example 1, except that 12.5g of polyvinyl alcohol (hereinafter referred to as PVA (10)) having a saponification degree of 10% was used instead of 5.0g of PVA (80), and 27.0g of terpineol (hereinafter referred to as TP) (hereinafter referred to as MMB 11.0 g) and 10.0g of water were used instead of 34.0g of MMB and 20.0g of water.
Example 5
A p-type impurity diffusion composition 8 was obtained in the same manner as in example 4, except that 10.0g of polyvinyl alcohol (hereinafter referred to as PVA (49)) having a saponification degree of 49% was used instead of 12.5g of PVA (10).
Example 6
A p-type impurity diffusion composition 9 was obtained in the same manner as in example 1, except that 10.0g of PVA (49) was used instead of 5.0g of PVA (80), and that TP 27.0g, 1, 3-propanediol (hereinafter referred to as 1, 3-PD) 11.0g and water 10.0g were used instead of MMB 34.0g and water 20.0 g.
Example 7
A p-type impurity diffusion composition 10 was obtained in the same manner as in example 1, except that polyethylene glycol 400 (manufactured by tokyo chemical Co., ltd.) was used instead of PVA (80) and an organic filler B was used instead of organic filler a.
The p-type impurity diffusion compositions of examples 1 to 7 and comparative examples 1 to 3 obtained were evaluated in terms of (1) to (5). The evaluation results are shown in table 2.
TABLE 11
TABLE 2
Description of the reference numerals
1 Semiconductor substrate
2 Pattern of impurity diffusion composition film (a)
3 Gas containing impurity diffusion component
(B) (c) impurity diffusion layer
(D) Layer comprising silicon oxide
Claims (9)
1. A p-type impurity diffusion composition comprising (A) a group 13 element compound, (B) a hydroxyl group-containing polymer, and (C) an organic filler made of a polymer obtained by crosslinking.
2. The p-type impurity diffusion composition according to claim 1, wherein the organic filler (C) made of a crosslinked polymer has an ethylene oxide or a propylene oxide.
3. The p-type impurity diffusion composition according to claim 2, wherein the (C) organic filler made of a crosslinked polymer is a crosslinked product obtained by copolymerizing the following (C-1) compound with the (C-2) compound:
(C-1) a compound having at least 1 group selected from an acryl group and a methacryl group; and
(C-2) Compounds having an acryl group or a methacryl group bonded to both ends of a structure having an ethylene oxide or a propylene oxide.
4. The p-type impurity diffusion composition according to any one of claims 1 to 3, wherein the hydroxyl group-containing polymer (B) is polyvinyl alcohol.
5. The p-type impurity diffusion composition according to claim 4, wherein the polyvinyl alcohol has a saponification degree of 20 mol% or more and less than 70 mol%.
6. A p-type impurity diffusion composition according to any one of claims 1 to 3, which contains 1, 3-propanediol as a solvent.
7. A method for manufacturing a solar cell includes a step of forming an impurity diffusion layer at 2 or more levels of different impurity concentrations,
The forming of the impurity diffusion layer of at least 1 level or more includes the steps of:
A step of partially forming an impurity diffusion composition film (a) by applying the p-type impurity diffusion composition according to any one of claims 1 to 3 to a semiconductor substrate; and
And (b) heating the obtained impurity diffusion composition film (a) to diffuse the impurities into the semiconductor substrate and form an impurity diffusion layer (b).
8. The method for manufacturing a solar cell according to claim 7, comprising a step of diffusing an impurity into a portion where the impurity diffusion composition film (a) is not formed, using the impurity diffusion composition film (a) as a mask.
9. The method for manufacturing a solar cell according to claim 8, wherein the step of diffusing the impurity into the portion where the impurity diffusion composition film (a) is not formed is a step of heating in an atmosphere containing an impurity diffusion component.
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