CN104668572A - Silver powder and silver paste for back electrode of solar cell and solar cell - Google Patents
Silver powder and silver paste for back electrode of solar cell and solar cell Download PDFInfo
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- CN104668572A CN104668572A CN201310624310.6A CN201310624310A CN104668572A CN 104668572 A CN104668572 A CN 104668572A CN 201310624310 A CN201310624310 A CN 201310624310A CN 104668572 A CN104668572 A CN 104668572A
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Abstract
The invention provides silver powder for a back electrode of a solar cell. The silver powder is prepared by the steps of S10, adding ammonium hydroxide to a silver nitrate solution to obtain a silver-ammonia solution; S20, adding polyvinylpyrrolidone to the silver-ammonia solution to obtain a first solution; S30, adding polysorbate to a reducing agent solution to obtain a second solution; S40, dropwise adding the first solution to a second solution, ageing after reaction, separating solid and liquid, remaining the precipitate, and drying to obtain the silver powder for the rear electrode of the solar cell. The invention further provides silver paste containing the silver powder, and the solar cell prepared from the silver paste. The silver powder for the back electrode of the solar cell is small in particle size pan, high in particle dispersing performance, small in impure ion content, and high in batch repeatability; the silver paste for the back electrode of the solar cell adopting the silver paste is relatively high in conductive performance, and the photoelectric conversion efficiency of the solar cell can be effectively increased.
Description
Technical field
The invention belongs to technical field of solar batteries, particularly relate to a kind of back electrode of solar cell silver powder, back electrode of solar cell silver slurry and a kind of solar cell.
Background technology
Solar energy is a kind of green energy resource, is more and more subject to people's attention, so solar cell arises at the historic moment because it is pollution-free, inexhaustible, not by advantages such as resource advantage restrictions.Solar cell is a kind of semiconductor devices that solar energy can be converted to electric energy, and under the condition of illumination, solar cell can generation current, to be got up by electric collecting and transfer out by grid line and electrode.Rear surface of solar cell electrode and grid line all by conductive silver paste by sintering support after high accuracy printing.
At present, conventional back silver slurry used for solar batteries is main containing silver powder, glass dust and organic carrier, and wherein the performance of silver powder is particularly important.The key technical index such as the quality of silver slurry, the conductance after conductive silver paste film forming and compactness are all determined by the performance of silver powder.Preparation method at present about silver powder has many reports, and main method has spray pyrolysis, electrolysis, microwave method, plasma method, mechanochemical synthesis, chemical reduction method etc.Wherein chemical reduction method becomes the main method preparing silver powder at present because of advantages such as its experimental facilities are simple, easy to operate, cost is low, energy-conservation, it mainly adopts reducing agent to reduce silver nitrate in aqueous, washing after Separation of Solid and Liquid, drying, ball milling sieve, and obtain silver powder.But it is more to introduce auxiliary agent kind in chemical reduction method process, in subsequent ball milling process, also can introduce ball-milling medium impurity, cause impurity content in silver powder higher, and silver powder size distribution is uneven, easily reunites.
Summary of the invention
The invention solves the technical problem that higher, the easy reunion of impurity content in the silver powder existed in prior art causes quality of cathode silver low.
The invention provides a kind of back electrode of solar cell silver powder, the step preparing described back electrode of solar cell silver powder comprises:
S10, in liquor argenti nitratis ophthalmicus, add ammoniacal liquor, form silver ammino solution;
S20, in silver ammino solution, add polyvinylpyrrolidone, obtain the first solution;
S30, in reductant solution, add polysorbate, obtain the second solution;
S40, be added drop-wise in the second solution by the first solution, reaction terminates rear ageing, retains and will precipitate also drying, obtain described back electrode of solar cell silver powder after Separation of Solid and Liquid.
Present invention also offers a kind of back electrode of solar cell silver slurry, containing silver powder, glass dust and organic carrier in described back electrode of solar cell silver slurry; Described silver powder is back electrode of solar cell silver powder provided by the invention.
Finally, the invention provides a kind of solar cell, the preparation process of described solar cell comprises: at the back side of silicon chip successively printed back silver slurry and back field aluminum paste material, at silicon chip full wafer printing front side silver paste after oven dry, obtains described solar cell after entering continuous tunnel furnace sintering; Wherein, described back silver slurry is back electrode of solar cell silver slurry provided by the invention.
Back electrode of solar cell silver powder provided by the invention, it is prepared by silver mirror reaction, namely silver-colored predecessor is silver ammino solution, simultaneously by introducing polyvinylpyrrolidone (being called for short PVP) in silver ammino solution, introduce polysorbate (also known as tween) in reducing agent, by the duplicate protection of PVP and tween, effectively can prevent the reunion of silver powder in preparation process, there is good dispersiveness in product system, ensure to obtain the silver powder product that particle size span is narrow, Granular composite performance is high; Do not introduce other objectionable impurities simultaneously, effectively can improve the purity of silver powder product, ensure its high batch repeatability.Adopt the back electrode of solar cell of this silver powder silver slurry to have higher electric conductivity, effectively can improve the electricity conversion of solar cell.
Detailed description of the invention
The invention provides a kind of back electrode of solar cell silver powder, the step preparing described back electrode of solar cell silver powder comprises:
S10, in liquor argenti nitratis ophthalmicus, add ammoniacal liquor, form silver ammino solution;
S20, in silver ammino solution, add polyvinylpyrrolidone, obtain the first solution;
S30, in reductant solution, add polysorbate, obtain the second solution;
S40, be added drop-wise in the second solution by the first solution, reaction terminates rear ageing, retains and will precipitate also drying, obtain described back electrode of solar cell silver powder after Separation of Solid and Liquid.
Back electrode of solar cell silver powder provided by the invention, it is prepared by silver mirror reaction, namely silver-colored predecessor is silver ammino solution, simultaneously by introducing polyvinylpyrrolidone (being called for short PVP) in silver ammino solution, introduce polysorbate (also known as tween) in reducing agent, by the duplicate protection of PVP and tween, effectively can prevent the reunion of silver powder in preparation process, there is good dispersiveness in product system, ensure to obtain the silver powder product that particle size span is narrow, particle dispersion is high; Do not introduce other objectionable impurities simultaneously, effectively can improve the purity of silver powder product, ensure its high batch repeatability.
Particularly; in the present invention; described silver powder is by silver ammino solution reduction being prepared; from directly adopt reducing agent by different for silver nitrate reduction method in prior art; on the one hand; in silver ammino solution silver ion dispersion evenly; on the other hand; the reduction reaction of silver ammino solution is faster than the reduction reaction rate of silver nitrate; silver powder deposition velocity is fast; simultaneously in the present invention also by adding PVP and tween as duplicate protection, the reunion of silver particles can be prevented further, thus prepare the silver powder that particle size span is narrow, particle dispersion is high.
Particularly, in the present invention, described silver ammino solution obtains by adding ammoniacal liquor in liquor argenti nitratis ophthalmicus.The present inventor finds, silver ammino solution described in the present invention in the preparation, can only adopt ammoniacal liquor as compounding ingredient, when selecting other alkali, can introduce other foreign ion in system, be difficult to the purity ensureing silver powder, the alkalescence of other alkali also can cause reaction rate wayward too by force simultaneously.For ensureing carrying out smoothly of follow-up silver mirror reaction, under preferable case, the consumption of described ammoniacal liquor is make the pH value of described silver ammino solution be 8 ~ 9.Described ammoniacal liquor can adopt the ammoniacal liquor of 25 ~ 28wt%, but is not limited to this.
In the present invention, described liquor argenti nitratis ophthalmicus directly can adopt commercial products, and also can prepare by being dissolved in nitric acid by silver-colored simple substance, the present invention is not particularly limited.Under preferable case, the concentration of described liquor argenti nitratis ophthalmicus is 3.4 ~ 6.8g/L.
In the present invention, described reducing agent can adopt the various reducing agents being applicable to silver mirror reaction, and it by the anion reduction in silver-colored amine complex, such as, can adopt aldehydes, hydrazine hydrate or ascorbic acid.In the present invention, described reducing agent is for ascorbic acid, and the reduction reaction related to is:
2Ag(NH
3)
2 + + C
6H
8O
6 = 2Ag + 2NH
4 ++ C
6H
6O
6+ 2NH
3
In above formula, C
6h
8o
6be ascorbic acid, C
6h
6o
6for propylene-1,2,3-tricarboxylic acids (having another name called aconitic acid).
In the present invention, inventor, by testing discovery further, when ascorbic acid is used as the reducing agent, obtains quality of cathode silver higher, this is because the reduction intensity of ascorbic acid is compared to other conventional reducing agent milder, is conducive to the reduction reaction speed controlling reaction system; Therefore, in the present invention, described reducing agent preferably adopts ascorbic acid.The consumption of described reducing agent can be selected in right amount according to the stoichiometric proportion of silver mirror reaction, and under preferable case, the weight ratio of reducing agent and silver nitrate is (7 ~ 12): 100.
As previously mentioned, in the present invention, in silver ammino solution, add PVP, in reductant solution, add polysorbate, effectively can prevent the reunion of silver powder in preparation process.In the present invention, by adopting high molecular weight water soluble polymer PVP as protective agent simultaneously, lactam group wherein containing polarity in PVP molecule and nonpolar methylene, by the Atomic coordinate on nitrogen-atoms wherein and oxygen atom and silver particles surface, formation adsorption layer more closely; And its C-H long-chain stretches to surrounding, form steric barrier, effectively can stop the reunion around between other silver particles.Inventor finds, in reaction system of the present invention, the growth mechanism of silver particles may be made up of following 3 steps: the silver ion in (1) silver ammino solution and PVP first react, and its reaction is more thorough compared to the reaction of common silver ion and PVP; (2) silver ion in silver ammino solution is reduced to silver atoms and mutually in-plant silver atoms be combined with each other and forms initial silver particles, is also called primary particle; (3) primary particle and PVP continuation effect or form second particle with neighbouring primary particle continuation effect.Therefore PVP can play the effect of the silver particles in the reunion and stabilizing solution suppressing silver particles.Add polysorbate (i.e. tween) as non-ionic surface active agent simultaneously, its unionization and containing more hydrophilic group in water, general without hydrophobic group, therefore it has better stability and water-soluble compared with other surfactants, not easily by the impact of system Inner electrolysis matter and Acidity of Aikalinity.In addition, polysorbate is easy to set up hydrogen bond and affinity interaction between Argent grain, is adsorbed on Argent grain surface than being easier to, and repulsion can be provided like this to play sterically hindered effect again, thus play peptizaiton.Therefore, in the present invention, when adopting PVP jointly to add in reaction solution as non-ionic surface active agent as protective agent and tween; can silver particles in stabilizing solution suppress the agglomeration of silver particles further; make silver powder epigranular, span is narrow, and particle dispersion is high.
Under preferable case, in the present invention, the weight ratio of polyvinylpyrrolidone and silver nitrate is (6 ~ 9): 100.The weight ratio of polysorbate and silver nitrate is (20 ~ 30): 100.
As previously mentioned, in the present invention, described polysorbate is used as non-ionic surface active agent, and its Main Function is the Argent grain in dispersion.In the present invention, carry out the polysorbate adopted in replacing whole or Some substitute the present invention according to other common dispersant in prior art (such as polyethylene glycol (PEG), triton x-100 (Trion X-100) or triethanolamine (TEA)), the dispersiveness of Argent grain all can be caused to reduce.Accordingly, the photoelectric transformation efficiency of the solar cell adopting this silver powder to prepare also can be lower slightly.
In addition, as a kind of preferred embodiment of the present invention, for ensureing that in reaction system, each raw material can be uniformly dispersed, also comprise the step of the second solution being carried out to strong stirring, SZCL type series constant temperature blender with magnetic force such as can be adopted to carry out constant temperature stirring to the second solution, and mixing time is 40 ~ 60min.
In the present invention, after the first solution (silver ammino solution namely containing PVP) is dropped to the second solution (reductant solution namely containing tween), namely start in the second solution reduction reaction occurs, the anion in silver-colored amine complex is reduced into silver ion.Inventor finds, the quality of the silver powder operating procedure that the first solution is added dropwise to the second solution obtained in the present invention will apparently higher than the operating procedure be added dropwise to by the second solution in the first solution, this be due to by the second solution add in the first solution time, because amine complex silver-colored in the first solution is in excessive state relative to reducing agent, very easily reunite after its reduction forms silver particles, cause silver powder particle size span greatly to increase., the first solution is added dropwise in the second solution meanwhile, effectively can also ensures thoroughly carrying out of reduction reaction.
In the present invention, after the first solution is all dropped to the second solution, also need reaction system to carry out ageing, make reaction more thorough.Under preferable case, the time of described ageing is 2 ~ 5h.
According to the present invention, after ageing, Separation of Solid and Liquid can be carried out to product system, retain precipitation (i.e. Argent grain sediment) after separation, then drying is carried out to precipitation, namely obtain described back electrode of solar cell silver powder.Wherein the method for Separation of Solid and Liquid can adopt centrifugation, but is not limited to this.More preferably in situation, the rotating speed of centrifugation is 4000 ~ 6500 turns/min, and the temperature of centrifugation is 30 ~ 45 DEG C, and the time of centrifugation is 20 ~ 40min.
Precipitation can be proceeded in baking oven after separation and carry out drying.Under preferable case, dry temperature is 40 ~ 60 DEG C.After drying completes, namely obtain described back electrode of solar cell silver powder.Back electrode of solar cell silver powder provided by the invention, its particle size span is narrow, particle dispersion is high; And impurity content is low in this silver powder, batch repeatability is high, is applicable to make back electrode of solar cell silver slurry.
Therefore, invention further provides a kind of back electrode of solar cell silver slurry, containing silver powder, glass dust and organic carrier in described back electrode of solar cell silver slurry; Described silver powder is back electrode of solar cell silver powder provided by the invention.Adopt the back electrode of solar cell of silver powder provided by the invention silver slurry to have higher electric conductivity, effectively can improve the electricity conversion of solar cell.
In the present invention, in described back electrode of solar cell silver slurry, in the normal ranges of content each component in the common electrode slurry of this area of silver powder, glass dust, organic carrier, the present invention does not have particular/special requirement.As previously mentioned, the silver powder provided in the present invention, its even particle size distribution, tap density are suitable, and impurity content is low, therefore in silver slurry provided by the invention, the content of silver powder suitably can improve relative in existing electrode slurry, and silver powder reunion can not be there is, also ensure effective dispersiveness of silver slurry simultaneously, improve follow-up printing efficiency.Particularly, as a kind of preferred embodiment of the present invention, with the gross mass of described back electrode of solar cell silver slurry for benchmark, wherein the content of silver powder is 75 ~ 85wt%, and the content of glass dust is 10 ~ 15wt%, and the content of organic carrier is 5 ~ 10wt%.
In the present invention, described glass dust can adopt various solar battery electrode slurry glass dust common in prior art, and it is generally common burning oxide.Such as, described glass dust preferably can adopt SiO
2-Bi
2o
3-ZnO-B
2o
3system lead-free glass powder, its softening temperature is 500 ~ 700 DEG C, but is not limited to this.More preferably in situation, described SiO
2-Bi
2o
3-ZnO-B
2o
3the SiO of consisting of of system lead-free glass powder: 1 ~ 5wt%
2, 20 ~ 25wt% Bi
2o
3, the ZnO of 15 ~ 30wt% and the B of 40 ~ 60%
2o
3.In the present invention, described glass dust directly can adopt commercial products, but also oneself preparation, and preparation method is known to the skilled person.Such as, the method preparing described glass dust can be: adopt V-Mixer to be mixed by the material powder of each composition glass dust according to raw material composition, to proceed in corundum crucible and to be placed in silicon carbide rod furnace, be warming up to 550 DEG C, insulation 0.5h, be warming up to 1000 DEG C again, insulation 1h, shrend is filtered and is obtained bead; Then bead is loaded ball grinder, in mass ratio zirconia ball: bead: deionized water=4:1:0.7, tank speed 300 revs/min, first wet-milling 6.5h, filters post-drying, then the 0.5h that dry grinds, during dry grinding, the mass ratio of zirconia ball and glass dust is 1:2, obtains described glass dust.
In the present invention, described organic carrier can adopt various organic carriers conventional in existing back electrode silver slurry used for solar batteries, and the present invention is not particularly limited.Such as, organic solvent, thickener and auxiliary agent is contained in described organic carrier.Wherein, described organic solvent can adopt the combination of multi-solvents conventional in prior art, such as, can be selected from one or more in alcohol ester, terpinol, dibutyl phthalate (DBP), BC, turpentine oil, BC acetate, butyl glycol ether, ethylene glycol ether acetate.Described thickener be selected from ethyl cellulose, nitrocellulose, alkyd resins, phenolic resins class binding agent one or more.Described auxiliary agent be selected from polyamide powder, rilanit special, hexadecanol, octadecyl alcolol one or more.With the gross mass of described organic carrier for benchmark, it consists of: the organic solvent of 85 ~ 95wt%, the thickener of 3.0 ~ 10wt% and the auxiliary agent of 0.5 ~ 5.0wt%.Described organic carrier directly can adopt commercial products, but also oneself preparation, such as preparation method can be: be added in above-mentioned organic solvent by thickener, auxiliary agent, make it fully dissolve and stir at 50 ~ 70 DEG C, can obtain transparent homogeneous organic carrier.
Back electrode of solar cell silver slurry provided by the invention, prepare by following steps: comprise and first glass dust being first scattered in organic carrier, then add silver powder in batches, be ground to slurry fineness and be less than 5 μm, back electrode of solar cell of the present invention silver slurry can be obtained.
As previously mentioned, back electrode of solar cell silver slurry provided by the invention has higher electric conductivity, effectively can improve the electricity conversion of solar cell.Therefore, the present invention finally provides a kind of solar cell, the preparation process of described solar cell comprises: at the back side of silicon chip successively printed back silver slurry and back field aluminum paste material, at silicon chip full wafer printing front side silver paste after oven dry, obtains described solar cell after entering continuous tunnel furnace sintering; Wherein, described back silver slurry is back electrode of solar cell silver slurry provided by the invention.
In the present invention, described back field aluminum paste material and front side silver paste are the various conventional slurry that those skilled in the art commonly use, and the present invention is not particularly limited, and repeats no more herein.Described silicon chip can be monocrystalline silicon piece or polysilicon chip, and the present invention is not particularly limited.
Adopt back electrode of solar cell provided by the invention silver slurry to print silicon chip back side, backplate and grid line can be formed after follow-up sintering.Wherein, the mode of printing can adopt serigraphy, but is not limited to this.As the common practise of those skilled in the art, during serigraphy, the printing consumption of back silver slurry suitably can be selected according to the size of cell piece.
As previously mentioned, back electrode of solar cell silver slurry provided by the invention has wider high temperature sintering region, therefore, in the present invention, when preparing described solar cell, sintering temperature interval in continuous tunnel furnace is also corresponding is effectively widened, and in the present invention, the temperature range in described continuous tunnel furnace is 860 ~ 920 DEG C.
In order to make technical problem solved by the invention, technical scheme and beneficial effect clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
Embodiment 1
(1) preparing 1000mL concentration is the liquor argenti nitratis ophthalmicus of 3.75g/L, adding the ammoniacal liquor that concentration is 25wt%, to obtaining the silver ammino solution that pH is 8, then adding 0.3g polyvinylpyrrolidone (PVP), namely the weight ratio of silver nitrate and PVP is 100:8, obtains the first solution.
(2) by 0.4g dissolution of ascorbic acid in 40mL water, be mixed with in reductant solution, then in this solution, add 0.3g polysorbate (tween), adopt SZCL type series constant temperature blender with magnetic force constant temperature to stir 40min, obtain the second solution.
(3) under normal temperature, the first solution that step (1) obtains is added drop-wise in the second solution that step (2) obtains, after whole dropping terminates, reaction system is continued ageing 3h, then proceed in centrifuge tube and carry out high speed centrifugation separation (temperature is 30 DEG C, time is 30min, rotating speed is 6000 turns/min), be separated the precipitation obtained and proceed in 50 DEG C of vacuum drying chambers dry, obtain black powder, be the silver powder of the present embodiment, be designated as S1.
(4) according to quality than terpinol: the ratio of BC=70:30 mixes, and obtains mixed solvent.Get the mixed solvent of 93.5 mass parts, add the ethyl cellulose STD-100 (the Dow Chemical Company produces, and viscosity is 100) of 5.0 mass parts, the rilanit special of 0.5 mass parts, the hexadecanol of 1.0 mass parts, is heated to 65 DEG C, make it fully dissolve, and stir, obtain organic carrier.First by the glass dust (SiO of concrete composition 3wt%
2, 22wt% Bi
2o
3, 15wt% the B of ZnO and 60wt%
2o
3softening temperature is 650 DEG C) be scattered in organic carrier, by after add the silver powder S1 that step (1) prepares in batches, the weight ratio of silver powder, glass dust and organic carrier is 85:10:5, be ground to slurry fineness and be less than 5 μm, obtain the back electrode of solar cell silver slurry S10 of the present embodiment.
(5) polysilicon chip specification is: 156 × 156mm, and thickness is 200 μm (before corrosion), and before printing, thickness is 180 μm.After by silicon wafer wool making, PN junction processed, plating silicon nitride anti-reflecting film, first at the back electrode of solar cell silver slurry S10 of silicon chip back side screen printing step (4), dry, serigraphy back field aluminum paste (Taiwan large standing grain science and technology 108C aluminium paste) is adopted equally in the remaining shady face part of back of the body silver slurry, then at front side of silicon wafer printing front side silver paste (Dupont company, 17F silver slurry), enter in continuous tunnel furnace and dry sintering, obtain the finished product solar cell of the present embodiment, be designated as S11.
Embodiment 2
(1) preparing 1000mL concentration is the liquor argenti nitratis ophthalmicus of 5.1g/L, adding the ammoniacal liquor that concentration is 28wt%, to obtaining the silver ammino solution that pH is 9, then adding 0.4g polyvinylpyrrolidone (PVP), namely the weight ratio of silver nitrate and PVP is 100:7.84, obtains the first solution.
(2) by 0.5g dissolution of ascorbic acid in 40mL water, be mixed with in reductant solution, then in this solution, add 0.4g polysorbate (tween), adopt SZCL type series constant temperature blender with magnetic force constant temperature to stir 40min, obtain the second solution.
(3) under normal temperature, the first solution that step (1) obtains is added drop-wise in the second solution that step (2) obtains, after whole dropping terminates, reaction system is continued ageing 4h, then proceed in centrifuge tube and carry out high speed centrifugation separation (temperature is 30 DEG C, time is 30min, rotating speed is 6000 turns/min), be separated the precipitation obtained and proceed in 50 DEG C of vacuum drying chambers dry, obtain black powder, be the silver powder of the present embodiment, be designated as S2.
(4) according to quality than terpinol: the ratio of BC=70:30 mixes, and obtains mixed solvent.Get the mixed solvent of 93.5 mass parts, add the ethyl cellulose STD-100 (the Dow Chemical Company produces, and viscosity is 100) of 5.0 mass parts, the rilanit special of 0.5 mass parts, the hexadecanol of 1.0 mass parts, is heated to 65 DEG C, make it fully dissolve, and stir, obtain organic carrier.First by the glass dust (SiO of concrete composition 5wt%
2, 25wt% Bi
2o
3, 30wt% the B of ZnO and 40wt%
2o
3softening temperature is 700 DEG C) be scattered in organic carrier, by after add the silver powder S2 that step (1) prepares in batches, the weight ratio of silver powder, glass dust and organic carrier is 75:15:10, be ground to slurry fineness and be less than 5 μm, obtain the back electrode of solar cell silver slurry S20 of the present embodiment.
(5) polysilicon chip specification is: 156 × 156mm, and thickness is 200 μm (before corrosion), and before printing, thickness is 180 μm.After by silicon wafer wool making, PN junction processed, plating silicon nitride anti-reflecting film, first at the back electrode of solar cell silver slurry S20 of silicon chip back side screen printing step (4), dry, serigraphy back field aluminum paste (Taiwan large standing grain science and technology 108C aluminium paste) is adopted equally in the remaining shady face part of back of the body silver slurry, then at front side of silicon wafer printing front side silver paste (Dupont company, 17F silver slurry), enter in continuous tunnel furnace and dry sintering, obtain the finished product solar cell of the present embodiment, be designated as S22.
Embodiment 3
(1) preparing 1000mL concentration is the liquor argenti nitratis ophthalmicus of 6.8g/L, adding the ammoniacal liquor that concentration is 27wt%, to obtaining the silver ammino solution that pH is 8, then adding 0.5g polyvinylpyrrolidone (PVP), namely the weight ratio of silver nitrate and PVP is 100:7.4, obtains the first solution.
(2) by 0.5g dissolution of ascorbic acid in 40mL water, be mixed with in reductant solution, then in this solution, add 0.4g polysorbate (tween), adopt SZCL type series constant temperature blender with magnetic force constant temperature to stir 40min, obtain the second solution.
(3) under normal temperature, the first solution that step (1) obtains is added drop-wise in the second solution that step (2) obtains, after whole dropping terminates, reaction system is continued ageing 5h, then proceed in centrifuge tube and carry out high speed centrifugation separation (temperature is 30 DEG C, time is 30min, rotating speed is 6000 turns/min), be separated the precipitation obtained and proceed in 50 DEG C of vacuum drying chambers dry, obtain black powder, be the silver powder of the present embodiment, be designated as S3.
(4) according to quality than terpinol: the ratio of BC=70:30 mixes, and obtains mixed solvent.Get the mixed solvent of 93.5 mass parts, add the ethyl cellulose STD-100 (the Dow Chemical Company produces, and viscosity is 100) of 5.0 mass parts, the rilanit special of 0.5 mass parts, the hexadecanol of 1.0 mass parts, is heated to 65 DEG C, make it fully dissolve, and stir, obtain organic carrier.First by the glass dust (SiO of concrete composition 1wt%
2, 24wt% Bi
2o
3, the ZnO of 23wt% and the B of 52%
2o
3softening temperature is 650 DEG C) be scattered in organic carrier, by after add the silver powder S3 that step (1) prepares in batches, the weight ratio of silver powder, glass dust and organic carrier is 75:15:10, be ground to slurry fineness and be less than 5 μm, obtain the back electrode of solar cell silver slurry S30 of the present embodiment.
(5) polysilicon chip specification is: 156 × 156mm, and thickness is 200 μm (before corrosion), and before printing, thickness is 180 μm.After by silicon wafer wool making, PN junction processed, plating silicon nitride anti-reflecting film, first at the back electrode of solar cell silver slurry S30 of silicon chip back side screen printing step (4), dry, serigraphy back field aluminum paste (Taiwan large standing grain science and technology 108C aluminium paste) is adopted equally in the remaining shady face part of back of the body silver slurry, then at front side of silicon wafer printing front side silver paste (Dupont company, 17F silver slurry), enter in continuous tunnel furnace and dry sintering, obtain the finished product solar cell of the present embodiment, be designated as S33.
Embodiment 4
(1) preparing 1000mL concentration is the liquor argenti nitratis ophthalmicus of 3.4g/L, adding the ammoniacal liquor that concentration is 25wt%, to obtaining the silver ammino solution that pH is 9, then adding 0.204g polyvinylpyrrolidone (PVP), namely the weight ratio of silver nitrate and PVP is 100:6, obtains the first solution.
(2) by 0.4g dissolution of ascorbic acid in 40mL water, be mixed with in reductant solution, then in this solution, add 0.68g polysorbate (tween), adopt SZCL type series constant temperature blender with magnetic force constant temperature to stir 40min, obtain the second solution.
(3) under normal temperature, the first solution that step (1) obtains is added drop-wise in the second solution that step (2) obtains, after whole dropping terminates, reaction system is continued ageing 2h, then proceed in centrifuge tube and carry out high speed centrifugation separation (temperature is 30 DEG C, time is 30min, rotating speed is 6000 turns/min), be separated the precipitation obtained and proceed in 50 DEG C of vacuum drying chambers dry, obtain black powder, be the silver powder of the present embodiment, be designated as S4.
(4) according to quality than terpinol: the ratio of BC=70:30 mixes, and obtains mixed solvent.Get the mixed solvent of 93.5 mass parts, add the ethyl cellulose STD-100 (the Dow Chemical Company produces, and viscosity is 100) of 5.0 mass parts, the rilanit special of 0.5 mass parts, the hexadecanol of 1.0 mass parts, is heated to 65 DEG C, make it fully dissolve, and stir, obtain organic carrier.First by the glass dust (SiO of concrete composition 5wt%
2, 20wt% Bi
2o
3, 25wt% the B of ZnO and 50wt%
2o
3softening temperature is 650 DEG C) be scattered in organic carrier, by after add the silver powder S4 that step (1) prepares in batches, the weight ratio of silver powder, glass dust and organic carrier is 85:10:5, be ground to slurry fineness and be less than 5 μm, obtain the back electrode of solar cell silver slurry S40 of the present embodiment.
(5) polysilicon chip specification is: 156 × 156mm, and thickness is 200 μm (before corrosion), and before printing, thickness is 180 μm.After by silicon wafer wool making, PN junction processed, plating silicon nitride anti-reflecting film, first at the back electrode of solar cell silver slurry S40 of silicon chip back side screen printing step (4), dry, serigraphy back field aluminum paste (Taiwan large standing grain science and technology 108C aluminium paste) is adopted equally in the remaining shady face part of back of the body silver slurry, then at front side of silicon wafer printing front side silver paste (Dupont company, 17F silver slurry), enter in continuous tunnel furnace and dry sintering, obtain the finished product solar cell of the present embodiment, be designated as S44.
Embodiment 5
(1) preparing 1000mL concentration is the liquor argenti nitratis ophthalmicus of 3.4g/L, adding the ammoniacal liquor that concentration is 25wt%, to obtaining the silver ammino solution that pH is 8, then adding 0.306g polyvinylpyrrolidone (PVP), namely the weight ratio of silver nitrate and PVP is 100:9, obtains the first solution.
(2) by 0.4g dissolution of ascorbic acid in 40mL water, be mixed with in reductant solution, then in this solution, add 1.02g polysorbate (tween), adopt SZCL type series constant temperature blender with magnetic force constant temperature to stir 40min, obtain the second solution.
(3) under normal temperature, the first solution that step (1) obtains is added drop-wise in the second solution that step (2) obtains, after whole dropping terminates, reaction system is continued ageing 3h, then proceed in centrifuge tube and carry out high speed centrifugation separation (temperature is 30 DEG C, time is 30min, rotating speed is 6000 turns/min), be separated the precipitation obtained and proceed in 40 DEG C of vacuum drying chambers dry, obtain black powder, be the silver powder of the present embodiment, be designated as S5.
(4) according to quality than terpinol: the ratio of BC=70:30 mixes, and obtains mixed solvent.Get the mixed solvent of 93.5 mass parts, add the ethyl cellulose STD-100 (the Dow Chemical Company produces, and viscosity is 100) of 5.0 mass parts, the rilanit special of 0.5 mass parts, the hexadecanol of 1.0 mass parts, is heated to 65 DEG C, make it fully dissolve, and stir, obtain organic carrier.First by the glass dust (SiO of concrete composition 4wt%
2, 21wt% Bi
2o
3, 15wt% the B of ZnO and 60wt%
2o
3softening temperature is 650 DEG C) be scattered in organic carrier, by after add the silver powder S5 that step (1) prepares in batches, the weight ratio of silver powder, glass dust and organic carrier is 85:10:5, be ground to slurry fineness and be less than 5 μm, obtain the back electrode of solar cell silver slurry S50 of the present embodiment.
(5) polysilicon chip specification is: 156 × 156mm, and thickness is 200 μm (before corrosion), and before printing, thickness is 180 μm.After by silicon wafer wool making, PN junction processed, plating silicon nitride anti-reflecting film, first at the back electrode of solar cell silver slurry S50 of silicon chip back side screen printing step (4), dry, serigraphy back field aluminum paste (Taiwan large standing grain science and technology 108C aluminium paste) is adopted equally in the remaining shady face part of back of the body silver slurry, then at front side of silicon wafer printing front side silver paste (Dupont company, 17F silver slurry), enter in continuous tunnel furnace and dry sintering, obtain the finished product solar cell of the present embodiment, be designated as S55.
Embodiment 6
(1) preparing 1000mL concentration is the liquor argenti nitratis ophthalmicus of 3.4g/L, adding the ammoniacal liquor that concentration is 25wt%, to obtaining the silver ammino solution that pH is 9, then adding 0.306g polyvinylpyrrolidone (PVP), namely the weight ratio of silver nitrate and PVP is 100:9, obtains the first solution.
(2) 0.4g hydrazine hydrate is dissolved in 40mL water, is mixed with in reductant solution, then in this solution, add 0.3g polysorbate (tween), adopt SZCL type series constant temperature blender with magnetic force constant temperature to stir 40min, obtain the second solution.
(3) under normal temperature, the first solution that step (1) obtains is added drop-wise in the second solution that step (2) obtains, after whole dropping terminates, reaction system is continued ageing 3h, then proceed in centrifuge tube and carry out high speed centrifugation separation (temperature is 30 DEG C, time is 30min, rotating speed is 6000 turns/min), be separated the precipitation obtained and proceed in 60 DEG C of vacuum drying chambers dry, obtain black powder, be the silver powder of the present embodiment, be designated as S6.
(4) according to quality than terpinol: the ratio of BC=70:30 mixes, and obtains mixed solvent.Get the mixed solvent of 93.5 mass parts, add the ethyl cellulose STD-100 (the Dow Chemical Company produces, and viscosity is 100) of 5.0 mass parts, the rilanit special of 0.5 mass parts, the hexadecanol of 1.0 mass parts, is heated to 65 DEG C, make it fully dissolve, and stir, obtain organic carrier.First by the glass dust (SiO of concrete composition 4wt%
2, 21wt% Bi
2o
3, 15wt% the B of ZnO and 60wt%
2o
3softening temperature is 650 DEG C) be scattered in organic carrier, by after add the silver powder S6 that step (1) prepares in batches, the weight ratio of silver powder, glass dust and organic carrier is 85:10:5, be ground to slurry fineness and be less than 5 μm, obtain the back electrode of solar cell silver slurry S60 of the present embodiment.
(5) polysilicon chip specification is: 156 × 156mm, and thickness is 200 μm (before corrosion), and before printing, thickness is 180 μm.After by silicon wafer wool making, PN junction processed, plating silicon nitride anti-reflecting film, first at the back electrode of solar cell silver slurry S60 of silicon chip back side screen printing step (4), dry, serigraphy back field aluminum paste (Taiwan large standing grain science and technology 108C aluminium paste) is adopted equally in the remaining shady face part of back of the body silver slurry, then at front side of silicon wafer printing front side silver paste (Dupont company, 17F silver slurry), enter in continuous tunnel furnace and dry sintering, obtain the finished product solar cell of the present embodiment, be designated as S66.
Embodiment 7
(1) preparing 100mL concentration is the liquor argenti nitratis ophthalmicus of 3.4g/L, adding the ammoniacal liquor that concentration is 25wt%, to obtaining the silver ammino solution that pH is 9, then adding 0.306g polyvinylpyrrolidone (PVP), namely the weight ratio of silver nitrate and PVP is 100:9, obtains the first solution.
(2) 0.4g hydrazine hydrate is dissolved in 40mL water, be mixed with in reductant solution, then in this solution, add 0.3g polysorbate (tween) and 0.45g polyethylene glycol (PEG), adopt SZCL type series constant temperature blender with magnetic force constant temperature to stir 40min, obtain the second solution.
(3) under normal temperature, the first solution that step (1) obtains is added drop-wise in the second solution that step (2) obtains, after whole dropping terminates, reaction system is continued ageing 3h, then proceed in centrifuge tube and carry out high speed centrifugation separation (temperature is 30 DEG C, time is 30min, rotating speed is 6000 turns/min), be separated the precipitation obtained and proceed in 50 DEG C of vacuum drying chambers dry, obtain black powder, be the silver powder of the present embodiment, be designated as S7.
(4) according to quality than terpinol: the ratio of BC=70:30 mixes, and obtains mixed solvent.Get the mixed solvent of 93.5 mass parts, add the ethyl cellulose STD-100 (the Dow Chemical Company produces, and viscosity is 100) of 5.0 mass parts, the rilanit special of 0.5 mass parts, the hexadecanol of 1.0 mass parts, is heated to 65 DEG C, make it fully dissolve, and stir, obtain organic carrier.First by the glass dust (SiO of concrete composition 4wt%
2, 21wt% Bi
2o
3, 15wt% the B of ZnO and 60wt%
2o
3softening temperature is 650 DEG C) be scattered in organic carrier, by after add the silver powder S7 that step (1) prepares in batches, the weight ratio of silver powder, glass dust and organic carrier is 85:10:5, be ground to slurry fineness and be less than 5 μm, obtain the back electrode of solar cell silver slurry S70 of the present embodiment.
(5) polysilicon chip specification is: 156 × 156mm, and thickness is 200 μm (before corrosion), and before printing, thickness is 180 μm.After by silicon wafer wool making, PN junction processed, plating silicon nitride anti-reflecting film, first at the back electrode of solar cell silver slurry S70 of silicon chip back side screen printing step (4), dry, serigraphy back field aluminum paste (Taiwan large standing grain science and technology 108C aluminium paste) is adopted equally in the remaining shady face part of back of the body silver slurry, then at front side of silicon wafer printing front side silver paste (Dupont company, 17F silver slurry), enter in continuous tunnel furnace and dry sintering, obtain the finished product solar cell of the present embodiment, be designated as S77.
Comparative example 1
Adopt the step (1-3) identical with embodiment 1 to prepare silver powder D1, difference is: step only prepares silver ammino solution in (1), and does not add PVP; Then in step (3), this silver ammino solution is dropped in the second solution.
(2) the back electrode of solar cell silver adopting the step (4) identical with embodiment 1 to prepare this comparative example starches D10, and difference is, adopts the silver powder S1 in silver powder D1 alternate embodiment 1.
(3) adopt the step (5) identical with embodiment 1 to prepare the solar cell D11 of this comparative example, difference is, adopts the back electrode of solar cell silver slurry S10 in back electrode of solar cell silver slurry D10 alternate embodiment 1.
Comparative example 2
Adopt the step (1-3) identical with embodiment 1 to prepare silver powder D2, difference is: step only prepares reductant solution in (2), and does not add polysorbate; Then in step (3), the first solution is directly dropped to not containing in the reductant solution of polysorbate.
(2) the back electrode of solar cell silver adopting the step (4) identical with embodiment 1 to prepare this comparative example starches D20, and difference is, adopts the silver powder S1 in silver powder D2 alternate embodiment 1.
(3) adopt the step (5) identical with embodiment 1 to prepare the solar cell D22 of this comparative example, difference is, adopts the back electrode of solar cell silver slurry S10 in back electrode of solar cell silver slurry D20 alternate embodiment 1.
Comparative example 3
The step (1-3) identical with embodiment 1 is adopted to prepare silver powder D3, difference is: only preparing 1000mL concentration in step (1) is 3.4g/L liquor argenti nitratis ophthalmicus, then 0.3g polyvinylpyrrolidone (PVP) is added, namely the weight ratio of silver nitrate and PVP is 100:8.8, obtains the first solution; Then in step (3), this first solution (liquor argenti nitratis ophthalmicus namely containing PVP) is dropped in the second solution.
(2) the back electrode of solar cell silver adopting the step (4) identical with embodiment 1 to prepare this comparative example starches D30, and difference is, adopts the silver powder S1 in silver powder D3 alternate embodiment 1.
(3) adopt the step (5) identical with embodiment 1 to prepare the solar cell D33 of this comparative example, difference is, adopts the back electrode of solar cell silver slurry S10 in back electrode of solar cell silver slurry D30 alternate embodiment 1.
Performance test
1, silver powder size distribution: adopt LS-POP(VI) laser particle size analysis tester silver powder S1-S7 and D1-D3 is analyzed.
2, silver slurry conducting performance test: adopt SZT-F type photovoltaic cell four pin tester to carry out test analysis to solar cell S11-S77 and D11-D33, record the resistivity of the back electrode that each cell piece back silver slurry is formed.
3, single flash operation simulation test instrument is adopted to carry out test analysis to solar cell S11-S77 and D11-D33.Test condition is standard test condition (STC): light intensity: 1000W/m
2; Spectrum: AM1.5; Temperature: 25 DEG C.Method of testing is carried out according to IEC904-1.More than test repetition 200 times, record its mean value.
Test result is as shown in table 1 below.
Table 1
。
Note:
In table, particle diameter corresponding when the cumulative particle sizes distribution number of D10: one sample reaches 10%, the particle that namely particle diameter is less than it accounts for 10%.
Particle diameter corresponding when the cumulative particle sizes distribution number of D50: one sample reaches 50%, the particle that namely particle diameter is less than it accounts for 50%.
Particle diameter corresponding when the cumulative particle sizes distribution number of D90: one sample reaches 10%, the particle that namely particle diameter is less than it accounts for 90%.
As can be seen from the test result of upper table 1, back electrode of solar cell silver powder provided by the invention, its size distribution span is narrower, and particle dispersion is high, and the foreign ion of this silver powder is few, and batch repeatability is high.Adopt this silver powder to prepare silver slurry and there is higher electric conductivity, make the electricity conversion adopting this silver to starch the solar cell prepared be 14.42 ~ 17.03wt%, be obviously better than the sample of comparative example.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (11)
1. a back electrode of solar cell silver powder, is characterized in that, the step preparing described back electrode of solar cell silver powder comprises:
S10, in liquor argenti nitratis ophthalmicus, add ammoniacal liquor, obtain silver ammino solution;
S20, in silver ammino solution, add polyvinylpyrrolidone, obtain the first solution;
S30, in reductant solution, add polysorbate, obtain the second solution;
S40, be added drop-wise in the second solution by the first solution, reaction terminates rear ageing, retains and will precipitate also drying, obtain described back electrode of solar cell silver powder after Separation of Solid and Liquid.
2. back electrode of solar cell silver powder according to claim 1, is characterized in that, in step S10, the concentration of described liquor argenti nitratis ophthalmicus is 3.4 ~ 6.8g/L.
3. back electrode of solar cell silver powder according to claim 1 and 2, is characterized in that, in step S10, the pH value of described silver ammino solution is 8 ~ 9.
4. back electrode of solar cell silver powder according to claim 1, is characterized in that, in step S20, the weight ratio of polyvinylpyrrolidone and silver nitrate is (6 ~ 9): 100.
5. back electrode of solar cell silver powder according to claim 1, is characterized in that, in step S30, described reducing agent is ascorbic acid; And the weight ratio of reducing agent and silver nitrate is (7 ~ 12): 100.
6. back electrode of solar cell silver powder according to claim 1 or 5, it is characterized in that, in step S30, the weight ratio of polysorbate and silver nitrate is (20 ~ 30): 100.
7. back electrode of solar cell silver powder according to claim 1, is characterized in that, in step S40, the time of described ageing is 2 ~ 5h, and the method for described Separation of Solid and Liquid is centrifugation; The temperature of described drying is 40 ~ 60 DEG C.
8. a back electrode of solar cell silver slurry, is characterized in that, containing silver powder, glass dust and organic carrier in described back electrode of solar cell silver slurry; Described silver powder is the back electrode of solar cell silver powder described in any one of claim 1-7.
9. back electrode of solar cell silver slurry according to claim 8, it is characterized in that, with the gross mass of described back electrode of solar cell silver slurry for benchmark, wherein the content of silver powder is 75 ~ 85wt%, the content of glass dust is 10 ~ 15wt%, and the content of organic carrier is 5 ~ 10wt%.
10. back electrode of solar cell silver slurry according to claim 8, is characterized in that, the SiO of consisting of of described glass dust: 1 ~ 5wt%
2, 20 ~ 25wt% Bi
2o
3, the ZnO of 15 ~ 30wt% and the B of 40 ~ 60%
2o
3.
11. 1 kinds of solar cells, the preparation process of described solar cell comprises: at the back side of silicon chip successively printed back silver slurry and back field aluminum paste material, at silicon chip full wafer printing front side silver paste after oven dry, obtains described solar cell after entering continuous tunnel furnace sintering; It is characterized in that, described back silver slurry is the back electrode of solar cell silver slurry described in any one of claim 9-10.
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| CN109807351A (en) * | 2019-03-18 | 2019-05-28 | 扬州大学 | The preparation method of ultra-small grain size nano copper particle |
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| CN114743717A (en) * | 2022-04-15 | 2022-07-12 | 北京大学深圳研究生院 | Silver powder composed of three-dimensional granular crystal and two-dimensional flaky crystal and preparation method thereof |
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| CN112264629A (en) * | 2020-11-03 | 2021-01-26 | 成都市天甫金属粉体有限责任公司 | Preparation method and application of low-cost high-dispersion silver powder |
| CN113724913A (en) * | 2021-09-07 | 2021-11-30 | 赵庆亮 | Preparation method of high-dispersion silver powder and conductive silver paste for solar cell |
| CN114743717A (en) * | 2022-04-15 | 2022-07-12 | 北京大学深圳研究生院 | Silver powder composed of three-dimensional granular crystal and two-dimensional flaky crystal and preparation method thereof |
| CN116072350A (en) * | 2023-04-07 | 2023-05-05 | 江西理工大学南昌校区 | Method for preparing conductive silver paste for solar cell electrode in situ |
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