CN110391037A - It is used to form the composition of electrode, using electrode and solar battery made of it - Google Patents

It is used to form the composition of electrode, using electrode and solar battery made of it Download PDF

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Publication number
CN110391037A
CN110391037A CN201811557813.5A CN201811557813A CN110391037A CN 110391037 A CN110391037 A CN 110391037A CN 201811557813 A CN201811557813 A CN 201811557813A CN 110391037 A CN110391037 A CN 110391037A
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chemical formula
electrode
weight
composition
polymer
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CN110391037B (en
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河京珍
文成日
李汉松
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Changzhou Fusion New Material Co Ltd
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Samsung SDI Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/04—Frit compositions, i.e. in a powdered or comminuted form containing zinc
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/08—Frit compositions, i.e. in a powdered or comminuted form containing phosphorus
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/02—Frit compositions, i.e. in a powdered or comminuted form
    • C03C8/10—Frit compositions, i.e. in a powdered or comminuted form containing lead
    • C03C8/12—Frit compositions, i.e. in a powdered or comminuted form containing lead containing titanium or zirconium
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C8/00—Enamels; Glazes; Fusion seal compositions being frit compositions having non-frit additions
    • C03C8/14—Glass frit mixtures having non-frit additions, e.g. opacifiers, colorants, mill-additions
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L29/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
    • C08L29/02—Homopolymers or copolymers of unsaturated alcohols
    • C08L29/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L29/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
    • C08L29/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • C08L33/04—Homopolymers or copolymers of esters
    • C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
    • C08L33/08—Homopolymers or copolymers of acrylic acid esters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
    • C08L75/04—Polyurethanes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/14—Conductive material dispersed in non-conductive inorganic material
    • H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
    • H—ELECTRICITY
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    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/20—Conductive material dispersed in non-conductive organic material
    • H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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    • 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
    • H01L31/02—Details
    • H01L31/0224—Electrodes
    • H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
    • H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar 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
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    • Y02E10/50—Photovoltaic [PV] energy

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Abstract

The present invention discloses a kind of composition for being used to form electrode, electrode and solar battery.The composition for being used to form electrode includes: conductive powder；Frit；Organic bond comprising polymer, the polymer include the structural unit indicated by chemical formula 1；Block isocyanate compound is indicated by chemical formula 2；And solvent.Each substituent group of chemical formula 1 and chemical formula 2 is identical as in specific embodiment.

Description

It is used to form the composition of electrode, using electrode and solar battery made of it
Technical field
The invention discloses a kind of composition for being used to form electrode, use electrode and solar battery made of it.
Background technique
Solar battery is produced electricl energy using the photovoltaic effect for the p-n junction that the photon of daylight is converted into electricity.In the sun Can in battery, preceding electrode and rear electrode be respectively formed in the semiconductor substrate (semiconductor wafer) with p-n junction front surface and In rear surface.By enter substrate day photo-induced p-n junction photovoltaic effect, and by the photovoltaic effect of p-n junction generate electricity Son is provided via the electric current outside electrode flow direction.
Can be formed on a surface of the substrate by the composition for being used to form electrode, being patterned and being fired has in advance Determine the electrode of the solar battery of pattern.
The transfer efficiency of known solar cells improves in the following manner: improve the contact performance of electrode and substrate and because This makes contact resistance (Rc) and series resistance (Rs) minimize；Or the pattern line-width of screen mask is adjusted with organic material It is smaller, and therefore form filament and increase short circuit current (Isc).However, reducing the method for the line width of electrode pattern with screen mask It may result in series resistance (Rs) increase and deteriorate the continuous impressionability of fine pattern.
The composition for being used to form electrode includes organic vehicle to assign the viscosity and rheological charactristics that are suitable for printing, and And organic vehicle generally comprises organic bond and solvent.
The amount of organic bond can be increased or can be used the polymer with high molecular weight so as to increase dispersibility and Storage stability.
However, when increasing the amount of organic bond, resistance may also be will increase during electrode is formed, and when use When organic bond with high molecular weight, may due to viscosity increases and there are trailing phenomenon (tailing phenomenon) And the problem of printing defects, even if being at high shear rates also such.
Summary of the invention
One embodiment offer, which is used to form, is capable of forming high resolution fine pattern and improved print characteristics, dispersibility And the composition of the electrode of storage stability.
The offer of another embodiment is used to form electrode made of the composition of electrode.
Another embodiment provides a kind of solar battery comprising the electrode.
According to an embodiment, the composition for being used to form electrode includes: conductive powder；Frit；Having comprising polymer Machine adhesive, the polymer include the structural unit indicated by chemical formula 1；Block isocyanate compound (block Isocyanate compound), it is indicated by chemical formula 2；And solvent.
[chemical formula 1]
In chemical formula 1,
R1For linear chain or branched chain C1 to the C10 alkyl for being substituted or being unsubstituted,
X is 50 moles of % to 90 moles of %, and
Y is 10 moles of % to 50 moles of %.
[chemical formula 2]
In chemical formula 2,
BL is methyl ethyl ketone oxime (methylethyl ketoxime), caprolactam (caprolactam), 3,5- diformazan Base pyrazoles (3,5-dimethyl pyrazole), 1,2,4- triazole (1,2,4-triazole), imidazoles (imidazole), 2- fourth Ketone diethyl malonate (2-butanine diethyl malonate) or ethyl acetoacetic ester (ethylacetoacetate), and
R2For linear chain or branched chain C1 to the C10 alkyl for being substituted or being unsubstituted.
Organic bond comprising polymer (including the structural unit indicated by chemical formula 1) with indicated by chemical formula 2 The mixed weight ratio of block isocyanate compound can be in the range of 30:1 to 1:1.
Polymer comprising the structural unit indicated by chemical formula 1 can further include the structural unit indicated by chemical formula 3.
[chemical formula 3]
In chemical formula 3,
R3For hydrogen or methyl,
R4For linear chain or branched chain C1 to the C10 alkyl for being substituted or being unsubstituted, and
Z is 0.01 mole of % to 30 moles of %.
With 100 moles of % comprising the polymer weight of the structural unit indicated by chemical formula 1, the knot indicated by chemical formula 3 The content of structure unit can be 0.1 mole of % to 30 moles of %.
The weight average molecular weight (Mw) of polymer comprising the structural unit indicated by chemical formula 1 can be 1,000 grams/mol (g/mol) to 300,000 grams/mol.
The composition for being used to form electrode may include conductive powder of the 60 weight % to 95 weight %；0.5 weight % to 20 The frit of weight %；The organic bond comprising polymer of 1 weight % to 20 weight %, the polymer include by chemistry The structural unit that formula 1 indicates；0.1 weight % is to the block isocyanate compound indicated to 5 weight % by chemical formula 2；And Solvent described in surplus.
Frit may include at least one element by selecting in the following terms: lead (Pb), tellurium (Te), bismuth (Bi), lithium (Li), phosphorus (P), germanium (Ge), gallium (Ga), cerium (Ce), iron (Fe), silicon (Si), zinc (Zn), tungsten (W), magnesium (Mg), caesium (Cs), strontium (Sr), molybdenum (Mo), titanium (Ti), tin (Sn), indium (In), vanadium (V), barium (Ba), nickel (Ni), copper (Cu), sodium (Na), potassium (K), arsenic (As), cobalt (Co), zirconium (Zr), manganese (Mn) and aluminium (Al).
Solvent may include at least one by selecting in the following terms: methyl cellosolve (methyl cellosolve), second Base cellosolve (ethyl cellosolve), butyl cellosolve (butyl cellosolve), fatty alcohol (aliphatic Alcohol), alpha-terpineol (α-terpineol), beta-terpineol (β-terpineol), dihydro-terpinol (dihydro- Terpineol), ethylene glycol (ethylene glycol), ethylene glycol monobutyl ether (ethylene glycol mono butyl Ether), butyl cellosolve acetate (butyl cellosolve acetate) and 2,2,4- trimethyl -1,3- pentanediol Mono isobutyrate (safe Sa alcohol) (2,2,4-trimethyl-1,3-pentanediol monoisobutyrate, Texanol).
The composition for being used to form electrode can further include at least one additive by selecting in the following terms: surface treatment Agent, dispersing agent, thixotropic agent, viscosity stabiliser, plasticiser, defoaming agent, pigment, ultraviolet light (ultraviolet；UV) stabilizer, Antioxidant and coupling agent.
The offer of another embodiment is used to form electrode made of the composition of electrode.
Another embodiment provides a kind of solar battery comprising the electrode.
The composition for being used to form electrode is capable of forming with high-resolution fine pattern and can have improved printing Feature, dispersibility and storage stability.
Detailed description of the invention
Fig. 1 is the schematic diagram for showing the structure of the solar battery according to one embodiment.
Drawing reference numeral explanation
100: substrate
101:p layers (or n-layer)
102:n layers (or p layers)
210: rear electrode
230: preceding electrode
Specific embodiment
Hereinafter, it is described more fully hereinafter with the disclosure with reference to the accompanying drawings, shows this hair in the drawings Bright exemplary embodiment.Such as those skilled in the art will recognize that, described reality can be modified in a variety of different ways Example is applied, these modifications all carry out without departing from the spirit or scope of the present invention.
In the accompanying drawings, the thickness in amplification layer, film, panel, region etc. for clarity.It is identical attached through this specification Figure grade indicates identical element.It should be understood that ought such as layer, film, region or substrate an element be referred to as " " another , can directly on the other element when element "upper", or there may also be insertion elements.In contrast, when element is claimed When element "upper" another for " directly existing ", insertion element is not present.
In the present specification, when in addition not providing specific definitions, " being substituted " refers at least one hydrogen via following The substituent group displacement selected in: halogen (F, Cl, Br or I), hydroxyl, C1 to C20 alkoxy, nitro, cyano, amino, imido Base, azido, amidino groups, diazanyl, hydrazono-, carbonyl, carbamyl, mercapto, ester group, ether, carboxyl or its salt, sulfonic group or Its salt, phosphate or its salt, C1 to C20 alkyl, C2 to C20 alkenyl, C2 to C20 alkynyl, C6 to C30 aryl, C3 to C20 cycloalkanes Base, C3 to C20 cycloalkenyl, C3 to C20 cycloalkynyl radical, C2 to C20 Heterocyclylalkyl, C2 to C20 heterocycloalkenyl, C2 to C20 heterocycle alkyne Base, C3 to C30 heteroaryl, or combinations thereof.
In the present specification, when in addition not providing specific definitions, term " miscellaneous " can refer to an original in cyclic substituents Son through N, O, S and P at least one hetero atom replace rather than at least one C replace the case where.
According to the composition for being used to form electrode of one embodiment include conductive powder, frit, organic bond with And solvent.
Hereinafter, the present invention will be described in detail.
The composition for being used to form electrode can be used metal powder as conductive powder.Metal powder may include by following At least one metal selected in: silver (Ag), gold (Au), palladium (Pd), platinum (Pt), ruthenium (Ru), rhodium (Rh), osmium (OS), iridium (Ir), rhenium (Re), titanium (Ti), niobium (Nb), tantalum (Ta), aluminium (Al), copper (Cu), nickel (Ni), molybdenum (Mo), vanadium (V), zinc (Zn), magnesium (Mg), yttrium (Y), cobalt (Co), zirconium (Zr), iron (Fe), tungsten (W), tin (Sn), chromium (Cr) and manganese (Mn), but not limited to this.
The granularity of conductive powder can be nanoscale or micron order.For example, the granularity of conductive powder can be received for tens Rice arrives several hundred nanometers or several microns to tens microns.In other embodiments, conductive powder can be with varigrained two Kind or more than two kinds of silver powder mixture.
Conductive powder can have spherical, slice-shaped or unbodied shape of particle.The average particle diameter of conductive powder (D50) 0.1 micron to 10 microns, such as 0.5 micron to 5 microns be can be.It can be under room temperature (20 DEG C to 25 DEG C) by super Sonicated disperses conductive powder in isopropanol (isopropyl alcohol, IPA) after 3 minutes, uses such as model 1064D (western Laeis GmbH (CILAS Co., Ltd.)) device measuring average particle diameter.Within the scope of these, composition It can provide low contact resistance and low line resistance.
In terms of the 100 weight % of total amount of composition for being used to form electrode, the content of conductive powder can be 60 weight % To 95 weight %.Within the scope of these, it can prevent transfer efficiency from deteriorating since resistance increases, and can also prevent by having Paste caused by the opposite reduction of machine mediator is difficult to be formed.In one embodiment, the amount of conductive powder may include 70 weights Measure % to 90 weight %.
Frit can be by etching anti-reflecting layer and melting conductive powder to enhance conductive powder and chip or lining Bonding force between bottom and the silver-colored crystal grain of formation in emitter region, thus in the firing work for the composition for being used to form electrode Reduce contact resistance during skill.In addition, frit can soften and can reduce firing temperature during sintering process.
When increasing the area of solar battery to improve solar battery efficiency, there are the contact of solar battery electricity A possibility that resistance may increase.Therefore, it is necessary to minimize the influence to p-n junction, while minimizing series resistance.In addition, with The purposes of various chips with different sheet resistances increases, and firing temperature can change in broad range.Need frit Ensure enough thermal stability to be resistant to broad range of firing temperature.
Frit can be one of the lead glass material being typically formed in the composition of electrode and non-lead frit Or it is a variety of.
Glass powder may include at least one metallic element by selecting in the following terms: lead (Pb), tellurium (Te), bismuth (Bi), lithium (Li), phosphorus (P), germanium (Ge), gallium (Ga), cerium (Ce), iron (Fe), silicon (Si), zinc (Zn), tungsten (W), magnesium (Mg), caesium (Cs), strontium (Sr), molybdenum (Mo), titanium (Ti), tin (Sn), indium (In), vanadium (V), barium (Ba), nickel (Ni), copper (Cu), sodium (Na), potassium (K), arsenic (As), cobalt (Co), zirconium (Zr), manganese (Mn) and aluminium (Al).
Frit can be prepared by any universal method by the oxide of metallic element.For example, metal oxide It can obtain in the following manner: with the oxide of estimated rate mixed metal element, melt mixture, gains are carried out Quenching, and then crush the product being quenched.Ball mill can be used or planetary mill carries out hybrid technique.Smelting process It can be carried out at 700 DEG C to 1300 DEG C, and quenching can carry out under room temperature (20 DEG C to 25 DEG C).Can be used disc mill or Planetary mill carries out disintegrating process, but not limited to this.
The average particle diameter (D50) of frit can be 0.1 micron to 10 microns, and to be used to form the combination of electrode The 100 weight % of total amount of object is counted, and content can be 0.5 weight % to 20 weight %.Within the scope of these, frit can be not The electrical characteristics of electrode are made to ensure the splendid adhesion strength of electrode of solar battery while deterioration.
Frit can have spherical form or amorphous shape.In one embodiment, can be used has different turn Two kinds of different classes of frits of temperature.For example, transition temperature is being greater than or equal to 200 DEG C to being less than or equal to The first frit and transition temperature within the scope of 350 DEG C are being higher than 350 DEG C of second glass within the scope of less than or equal to 550 DEG C Material can be mixed with the weight ratio of 1:0.2 to 1:1.
The composition for being used to form electrode may include polymer as organic bond, and the polymer includes by chemistry The structural unit that formula 1 indicates.
[chemical formula 1]
In chemical formula 1,
R1For linear chain or branched chain C1 to the C10 alkyl for being substituted or being unsubstituted,
X is 50 moles of % to 90 moles of %, and
Y is 10 moles of % to 50 moles of %.
Polymer comprising the structural unit indicated by chemical formula 1 has polyvinyl acetal structure (polyvinyl Acetal structure) and polyvinyl alcohol structures (polyvinyl alcohol structure).Polyvinyl acetal is usually logical It crosses and uses vinyl alcohol polymer as raw material to prepare.Polyvinyl alcohol can obtain in conventional manner, that is, by making vinyl acetate Class monomer polymerization is simultaneously saponified polymer obtained.The polymerization of vinyl esters monomer may include conventional method, such as molten Liquid polymerization, bulk polymerization, suspension polymerization, emulsion polymerisation process etc..Herein, polymerization side is depended on Method, polymerization initiator can properly be selected from azo-initiator, peroxide type initiators, redox type initiators etc. Deng.It can be routinely saponified using the alcoholysis of well-known alkali metal or acid catalyst, hydrolysis etc. by application, but In these methods, it is simple and most preferably for using methanol to carry out saponification as catalyst as solvent and sodium hydroxide (NaOH) 's.
Polyvinyl alcohol for the raw material as polyvinyl acetal (polyvinylacetal) of the invention, which can have, to be depended on In the average degree of polymerization that its purposes properly selects, but preferably 150 to 3,000 and more preferably 200 to 2, In the range of 000.
Acid catalyst for acetalation is not particularly limited, but may include any in organic acid and inorganic acid It is a, such as acetic acid, p-methyl benzenesulfonic acid (paratoluenesulfonic acid), nitric acid, sulfuric acid, hydrochloric acid etc..Wherein, preferably Using hydrochloric acid, sulfuric acid and nitric acid, and specifically, hydrochloric acid is more preferably used.
Aldehyde for acetalation of the invention is not particularly limited, but it is preferable to use the aldehyde acetals for being 1 to 8 by carbon number The polyvinyl acetal of change.The aldehyde that carbon number is 1 to 8 can be formaldehyde, acetaldehyde, propionic aldehyde, n-butanal, isobutylaldehyde, n-hexyl aldehyde, 2- ethyl Butyraldehyde, n-octaldehyde, 2- ethyl hexanal, benzaldehyde etc., the aldehyde can be used alone or as its at least two mixture It uses.Wherein, the aldehyde that carbon number is 4 to 6 is preferably n-butanal.
In other words, polyvinyl acetal is preferably polyvinyl butyral.
The average acetalation degree of polyvinyl acetal is preferably in the range of 40 moles of % to 85 moles of %, more preferably Ground is in the range of 48 moles of % to 82 moles of %, and even more preferably in the range of 55 moles of % to 81 moles of %.Separately Outside, in order to be appropriately carried out the purpose of the present invention, vinyl ester units content (generally, the vinyl acetate of polyvinyl acetal Unit content) it can range in the range of 0.01 mole of % to 30 moles of %, preferably in 0.05 mole of % to 15 moles of % It is interior, and more preferably in the range of 0.1 mole of % to 5 moles of %.In addition, vinyl alcohol units content can be arrived in 1 mole of % In the range of 50 moles of %, preferably in the range of 12 moles of % to 40 moles of %, and most preferably in 15 moles of % to 35 In the range of mole %.In addition, acetalation degree, vinyl ester units content and vinyl alcohol units content are based on acetalation journey Spend the summation of (ethylene acetal unit content), vinyl ester units content and vinyl alcohol units content.
In addition, the polymer comprising the structural unit indicated by chemical formula 1 can further include the structure list indicated by chemical formula 3 Member:
[chemical formula 3]
In chemical formula 3,
R3For hydrogen or methyl,
R4For linear chain or branched chain C1 to the C10 alkyl for being substituted or being unsubstituted, and
Z is 0.01 mole of % to 30 moles of %.
With 100 moles of % comprising the polymer weight of the structural unit indicated by chemical formula 1, the knot indicated by chemical formula 3 The amount of structure unit may include 0.1 mole of % to 30 moles of %.When the structural unit of chemical formula 3 is included in the range, The dispersibility and print characteristics for being used to form the composition of electrode can be improved.
The weight average molecular weight (Mw) of polymer comprising the structural unit indicated by chemical formula 1 can for 1,000 grams/mol to 300,000 grams/mol.In the range, the dispersibility and print characteristics for being used to form the composition of electrode can be improved.
In addition, the composition for being used to form electrode may include the block isocyanate compound indicated by chemical formula 2.
[chemical formula 2]
In chemical formula 2,
BL is methyl ethyl ketone oxime, caprolactam, 3,5- dimethyl pyrazole, 1,2,4- triazole, imidazoles, 2- butanone malonic acid Diethylester or ethyl acetoacetic ester, and
R2For linear chain or branched chain C1 to the C10 alkyl for being substituted or being unsubstituted.
Specifically, showing splendid room temperature stability by the block isocyanate compound that chemical formula 2 indicates, and another Outside, the cross-linking reaction by isocyanates and organic bond under the drying temperature (250 DEG C to 400 DEG C) of silver paste is come control line Wide expansion, while the blocking agent of the blocked isocyanate dissociates (dissociation temperature: 100 DEG C to 200 DEG C), and has and pass through Urethane bond (urethane bond) adheres to the improvement of the silicon wafer as substrate.
Organic bond comprising polymer (including the structural unit indicated by chemical formula 1) with indicated by chemical formula 2 The mixed weight ratio of block isocyanate compound can be in 30:1 to 1:1, and definitely in the range of 10:1 to 1:1.In In the range, line width expansion can control, and the adhesiveness with silicon wafer can be improved.
Other than block isocyanate compound, the composition for being used to form electrode can also further include typical case as needed Additive, to enhance flow behavior, operational characteristic and stability.Additive may include surface treating agent, dispersing agent, thixotroping Agent, viscosity stabiliser, plasticiser, defoaming agent, pigment, ultraviolet light (UV) stabilizer, antioxidant, coupling agent etc., the addition Agent can be used alone or use as its mixture.
In terms of the total amount (100 weight %) for being used to form the composition of electrode, the amount of these additives may include 0.1 weight % is measured to 5 weight %, but this amount can according to need change.The composition for being used to form electrode can be considered in the amount of additive Print characteristics, dispersibility and storage stability select.
The composition for being used to form electrode may include conductive powder of the 60 weight % to 95 weight %；0.5 weight % to 20 The frit of weight %；The organic bond comprising polymer of 1 weight % to 20 weight %, the polymer include by chemistry The structural unit that formula 1 indicates；0.1 weight % is to the block isocyanate compound indicated by chemical formula 2 to 5 weight %；With And solvent described in surplus.In the range, the composition for being used to form electrode can have proper viscosity and prevent to substrate Adhesiveness deterioration, and be also possible to due to organic bond the uneven decomposition during firing with high resistance, and prevent Only electrode cracks during firing, disconnects, with pin hole etc..
The boiling point of solvent can be 100 DEG C or be higher than 100 DEG C, and solvent can be methyl cellosolve, ethyl cellosolve, Butyl cellosolve, fatty alcohol, alpha-terpineol, beta-terpineol, dihydro-terpinol, ethylene glycol, ethylene glycol monobutyl ether, butyl are molten Fine agent acetic acid esters and 2,2,4- trimethyl -1,3- pentanediol mono isobutyrate (safe Sa alcohol) (2,2,4-trimethyl-1,3- Pentanediol monoisobutyrate, Texanol), it can be used alone or made with the combination of two or more With.
In terms of the composition for being used to form electrode, the solvent of surplus may include, and to be used to form the composition of electrode 100 weight % of total amount meter, may include such as 1 weight % to the solvent of 30 weight %.In the range, it can be ensured that foot Enough adhesion strengths and splendid print characteristics.
According to another embodiment, the electrode made of the composition for being used to form electrode is provided.
According to another embodiment, the solar battery comprising the electrode is provided.
Referring to Fig. 1, illustrate the solar battery according to one embodiment.Fig. 1 is the sun shown according to one embodiment The schematic diagram of the structure of energy battery.
Referring to Fig. 1, the composition for being used to form electrode is printed on substrate 100, and the substrate includes p layers of (or n-layer) 101 As emitter and it is fired with electrode 210 and preceding electrode 230 after formation with n-layer (or p layers) 102.For example, it is used for institute The previous preparation step for stating rear electrode can carry out in the following manner: the composition for being used to form electrode is printed in chip It is in rear surface and 10 seconds to 60 seconds dry at 200 DEG C to 400 DEG C, and make it dry.Due to by being included in for shape At the organic bond in the composition of electrode containing polymer (including the structural unit indicated by chemical formula 1) and by chemical formula The paste that 2 blocked isocyanates indicated are mixed and prepared has splendid storage at room temperature ability, and therefore shows at room temperature No viscosity change etc. is shown, therefore when composition is printed and coated within the temperature range of 200 DEG C to 400 DEG C, in block Generated isocyanates can react with the hydroxyl with chemical formula 1 and form cross-linked structure during the dissociation of isocyanates.
In addition, the previous preparation step for the preceding electrode can carry out in the following manner: electrode will be used to form Composition be printed in the front surface of chip, and make it dry.Then, the preceding electrode 120 and the rear electrode 130 can To be fired 30 seconds to 210 seconds at 400 DEG C to 980 DEG C, preferably at 700 DEG C to 980 DEG C, to form preceding electrode and rear electricity Pole.
Hereinafter, the disclosure is described in more details in reference example.However, these examples be it is exemplary, And the present disclosure is not limited thereto.
The synthesis of polymer
<synthesis example 1>
6.5 gram of 5 weight % aqueous hydrochloric acid solution is added in the round-bottomed flask equipped with the condenser with nitrogen atmosphere Into 100 gram of 10 weight % polyvinyl alcohol (degree of polymerization: 1,700, Dc Chemical Co., Ltd. (OCI Company Ltd.)) aqueous solution, And (purity 99% pacifies laughable this organic chemistry (Acros by 1.5 grams of butyl aldehyde (butyl aldehyde) Organics)) be added to wherein to be used to react, while stirring aqueous solution (temperature maintains 50 DEG C).Gains are cooled to 30 DEG C, and 4.0 grams of butyl aldehyde are added to wherein.Then, mixture is again heated to 50 °, and then maintain 4 hours with Complete reaction.By being washed with distilled water by its polymer obtained to remove unreacted reactant and dry at low temperature to obtain weight The polyvinyl butyral copolymer (polyvinylbutyral copolymer) that molecular weight is 130,000 grams/mol.
<synthesis example 2>
The polyvinyl alcohol contracting fourth that weight average molecular weight is 200,000 grams/mol is obtained according to method identical with synthesis example 1 Aldehyde copolymer, but the polyvinyl alcohol (Dc Chemical Co., Ltd.) for the use of the degree of polymerization being wherein 5,000.
The synthesis of block isocyanate compound
<synthesis example 3>
By hexamethylene diisocyanate trimer (Hexamethylene diisocyanate trimer) (1 equivalent) It is placed in the round-bottomed flask equipped with the condenser of nitrogen atmosphere, by methyl ethyl ketone oxime (methylethyl ketoxime) (1.5 equivalent) is added to wherein and is reacted with it at 75 DEG C as blocking agent, confirms that isocyanate groups disappear with FT-IR (2270cm-1) to complete to react, and then butyl cellosolve acetate is added to wherein viscosity is adjusted to 40, 000cps/25 DEG C and obtain have chemical formula 2 structural unit block isocyanate compound.
It is used to form the preparation of the composition of electrode
<example 1>
The composition for being used to form electrode is prepared by the following method: will be according to 1.5 weights of synthesis example 1 at 50 DEG C It measures % copolymer and is completely dissolved in as organic bond as solvent according to 1.5 weight % copolymers of synthesis example 2 In 6.5 weight % butyl cellosolve acetates, and will be according to 1 weight % block isocyanate compound of synthesis example 3, flat 2.0 weight % lead glass material (lead glass, CI-124, the Pa Dike that particle diameter is 1.0 microns and transition temperature is 341 DEG C Lip river gray(Gy) Co., Ltd (Particlogy Co., Ltd.)), as 0.2 weight % dispersant B YK102 (Bi Kehua of additive Learn limited liability company (BYK-chemie GmbH)) and 0.3 weight % thixotropic agent Thixatrol ST (Hai Mingsi company (Elementis Co.)) and average particle diameter (D50) be 1.5 microns 87 weight % ball shape silver powders (AG-4-8, more watts Electron Material Co., Ltd (Dowa Electronics Materials Co., Ltd.)) it is added to wherein, and pinched with three rollers It is equably mixed and is dispersed by conjunction machine.
<example 2>
It is used to form the composition of electrode according to method identical with example 1 preparation, but is wherein used according to synthesis example 1 2 weight % copolymers and according to synthesis example 21 weight % copolymer as organic bond.
<example 3>
It is used to form the composition of electrode according to method identical with example 1 preparation, but is wherein used according to synthesis example 1 1 weight % copolymer and according to synthesis example 22 weight % copolymers as organic bond.
<comparative example 1>
The composition of electrode is used to form according to method identical with example 1 preparation, but wherein without using real according to synthesis The copolymer of example 1 and according to synthesis example 2 copolymer, but use 3 weight % cellulosic binders (STD 45, Tao Shiization Company (Dow Chemical Company)) polymer is as organic bond.
<comparative example 2>
The composition of electrode is used to form according to method identical with example 1 preparation, but wherein without using real according to synthesis The copolymer of example 1, according to synthesis example 2 copolymer and block isocyanate compound, but use 3 weight % celluloses Adhesive (STD 45, Dow Chemical) polymer is as organic bond and 7.5 weight % solvents.
<comparative example 3>
It is used to form the composition of electrode according to method identical with example 1 preparation, but does not use blocked isocyanate wherein Ester compounds, but use 7.5 weight % solvents.
Characteristic evaluation
(1) storage stability (%)
Be used to form the composition of electrode storage stability be according to its viscosity change ratio before storing and later, It is assessed according to formula 1, and result is illustrated in table 1.
[formula 1]
F0To be at 25 DEG C to exist later for composition 1 day that storage is used to form electrode under 50 ± 5% relative humidity The viscosity measured under room temperature (25 DEG C), and
F1To be after being stored under relative humidity 50 ± 5% at 25 DEG C composition 30 days that are used to form electrode in room The viscosity measured under warm (25 DEG C).
※ obtains viscosity measurement in the following manner: using viscosimeter, (HBDV-2+pro, Bu Luoke Field are engineered Laboratory (Brookfield Engineering Laboratories)) and SC4-14 rotation and SC4-6RP are installed on it Chamber, and then composition is sheared in advance 30 seconds under 25 DEG C and 10rpm.
(2) fine pattern is assessed
According to each composition for being used to form electrode of example 1 to example 3 and comparative example 1 to comparative example 3, for Screen mask is screen printing electrode pattern (finger-like bar) in the front surface of 90 ohm of poly- P-type silicon chip in sheet resistance, And it is then dried by using infrared drying stove.Then, the composition for being used to form the electrode comprising aluminium is printed It is dry in method same as above in the rear surface of chip, and then.Then, pass through via battery made by above-mentioned technique It is fired 30 seconds to 50 seconds at 400 DEG C to 950 DEG C using conveyor-type smelting furnace, and (MV technology is public by using EL tester Department (MV Tech Inc.)) number of line opening is counted to check whether made electrode (finger-like bar) breaks Even, and using the line width and thickness of VK equipment (VK9710, Keyemce company (KEYENCE Co.)) measuring electrode line, and It the results are shown in table 1.
* screen mask: SUS325 type/lotion thickness: 15 microns/finger-like bar line width: 45 microns, finger-like bar number: 80
[table 1]
Example 1 Example 2 Example 3 Comparative example 1 Comparative example 2 Comparative example 3
Storage stability (%) 5 5 5 5 4 4
Line width L1 (micron) after printing 61 60 58 59 60 63
Line width L2 (micron) after drying 63 62 60 61 66 71
Line width L3 (micron) after firing 64 62 60 63 68 73
Thickness D1 (micron) after firing 21 22 21 20 20 19
Line width △ (L1-L2) (micron) △2 △2 △2 △2 △6 △8
Aspect ratio (D1/L3) 0.328 0.355 0.350 0.317 0.294 0.260
Referring to table 1, and real 3 composition for being used to form electrode is compared compared with according to comparative example 1, is arrived according to example 1 The composition for being used to form electrode of example 3 shows the filament of the storage stability more improved He the electrode pattern being made from it It is wide.
Although describing the present invention in conjunction with practical exemplary embodiment is presently considered as, it should be appreciated that the present invention is unlimited In the disclosed embodiments, and on the contrary, including in the spirit and scope of the appended claims each the invention is intended to cover Kind modification and equivalent arrangements.

Claims (11)

1. a kind of composition for being used to form electrode, comprising:
Conductive powder；
Frit；
Organic bond, including polymer, the polymer include the structural unit indicated by chemical formula 1；
Block isocyanate compound is indicated by chemical formula 2；And
Solvent,
[chemical formula 1]
Wherein, in chemical formula 1,
R1For linear chain or branched chain C1 to the C10 alkyl for being substituted or being unsubstituted,
X is 50 moles of % to 90 moles of %, and
Y is 10 moles of % to 50 moles of %；
[chemical formula 2]
Wherein, in chemical formula 2,
BL is methyl ethyl ketone oxime, caprolactam, 3,5- dimethyl pyrazole, 1,2,4- triazole, imidazoles, 2- butanone malonic acid diethyl Ester or ethyl acetoacetic ester, and
R2For linear chain or branched chain C1 to the C10 alkyl for being substituted or being unsubstituted.
2. the composition according to claim 1 for being used to form electrode, including the described organic viscous of the polymer The mixed weight ratio of mixture and the block isocyanate compound indicated by chemical formula 2 is in the range of 30:1 to 1:1, institute Stating polymer includes the structural unit indicated by chemical formula 1.
3. the composition according to claim 1 for being used to form electrode, including the structure indicated by chemical formula 1 The polymer of unit further includes the structural unit indicated by chemical formula 3:
[chemical formula 3]
Wherein, in chemical formula 3,
R3For hydrogen or methyl,
R4For linear chain or branched chain C1 to the C10 alkyl for being substituted or being unsubstituted, and
Z is 0.01 mole of % to 30 moles of %.
4. the composition according to claim 3 for being used to form electrode, wherein with 100 moles of % including by chemical formula 1 The polymer weight of the structural unit indicated, the content of the structural unit indicated by chemical formula 3 are 0.1 mole of % To 30 moles of %.
5. the composition according to claim 1 for being used to form electrode, including the structure indicated by chemical formula 1 The weight average molecular weight of the polymer of unit is in the range of 1,000 grams/mol to 300,000 grams/mol.
6. the composition according to claim 1 for being used to form electrode, wherein the composition packet for being used to form electrode It includes:
The conductive powder of the 60 weight % to 95 weight %；
The frit of the 0.5 weight % to 20 weight %；
The organic bond including the polymer of 1 weight % to 20 weight %, the polymer include by chemical formula 1 The structural unit indicated；
The block isocyanate compound of 0.1 weight % to 5 weight % indicated by chemical formula 2；And
Solvent described in surplus.
7. the composition according to claim 1 for being used to form electrode, wherein the frit includes by the following terms At least one metallic element selected: lead, tellurium, bismuth, lithium, phosphorus, germanium, gallium, cerium, iron, silicon, zinc, tungsten, magnesium, caesium, strontium, molybdenum, titanium, tin, Indium, vanadium, barium, nickel, copper, sodium, potassium, arsenic, cobalt, zirconium, manganese and aluminium.
8. the composition according to claim 1 for being used to form electrode, wherein the solvent includes by selecting in the following terms Out at least one: methyl cellosolve, ethyl cellosolve, butyl cellosolve, fatty alcohol, alpha-terpineol, beta-terpineol, dihydro- Terpinol, ethylene glycol, ethylene glycol monobutyl ether, butyl cellosolve acetate and 2,2,4- trimethyl -1,3- pentanediol Dan Yi Butyrate.
9. the composition according to claim 1 for being used to form electrode, wherein being used to form the composition of electrode also Including at least one additive by being selected in the following terms: surface treating agent, dispersing agent, thixotropic agent, viscosity stabiliser, plasticizing Agent, defoaming agent, pigment, ultra-violet stabilizer, antioxidant and coupling agent.
10. a kind of electrode, the composition that electrode is used to form described in any one of claims 1 to 9 is made.
11. a kind of solar battery, including electrode described in any one of claim 10.
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