CN102351427B - Preparation technology of silver-coated glass powder for solar cell silver paste - Google Patents
Preparation technology of silver-coated glass powder for solar cell silver paste Download PDFInfo
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- CN102351427B CN102351427B CN 201110200609 CN201110200609A CN102351427B CN 102351427 B CN102351427 B CN 102351427B CN 201110200609 CN201110200609 CN 201110200609 CN 201110200609 A CN201110200609 A CN 201110200609A CN 102351427 B CN102351427 B CN 102351427B
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Abstract
The invention discloses a preparation technology of silver-coated glass powder for a solar cell silver paste, comprising the steps of coarsening of glass powder, activation and sensitization of glass powder, and silver coating of glass powder. When sintering the conductive silver paste produced by using the prepared silver-coated glass powder herein, the glass powder body is softened and melted at first to form the viscous and plastic flow of the nano silver film coated on the surface of the glass powder, finally, silver is carried to the silicon chip for recrystallization and growing and forms a good ohmic contact with the silicon chip directly, thus the contact resistance is lowered, the contact area is greatly increased, the conductivity is good, and a good effect on improving conversion efficiency of the solar cell is achieved. The invention has the advantages of simple process and convenient operation. According to the invention, silver is in good ohmic contact with the silicon chip in the prepared solar cell electrodes with using the solar cell silver paste prepared by using the prepared silver-coated glass powder, the conductivity is good, the contact area is greatly increased, and the conversion efficiency of the solar cell is effectively improved. The invention is suitable for industrial application.
Description
Technical field
Patent of the present invention relates to a kind of preparation method for the preparation of the conductive silver paste raw material, relates in particular to solar cell cell front side silver paste and back silver slurry wraps glass powder with silver preparation method.Belong to the sun power preparing technical field.
Background technology
21 century global energy present situation in short supply is more and more outstanding, people also recognize limitation, the finiteness and non-renewable of conventional energy resources gradually, add that conventional energy resources causes serious destruction to environment, so that the development and utilization to new forms of energy has all been stepped up in countries in the world, sun power is energy that has development prospect in the new forms of energy, solar cell power generation is compared with the conventional power generation usage mode, it is pollution-free, noiselessness, safe and reliable, safeguard simple, the construction period is short, possibility with large-scale application.
The preparation technology of solar cell is ripe in the world at present, and conductive silver paste is prepared into the electrode of solar cell by silk screen printing, oven drying at low temperature, high-sintering process.Conductive silver paste mainly is prepared from by different proportionings by starting material such as silver powder, glass powder, organic carriers.Wherein silver powder is as conductive phase; Glass powder melts in sintering process as Binder Phase, silver powder is taken on the silicon substrate form ohmic contact with silicon; Organic carrier plays interim bonding, so that slurry is difficult for precipitation and oxidation in the preservation process, easily volatilizees when high temperature.The efficiency of conversion of solar cell and the resistance of the string of solar cell are closely bound up, in order to improve the efficiency of conversion of solar cell, prepare in the process of solar cell in reality, want the series resistance of reduce solar cell, the resistance of the string of solar cell mainly comprises the contact resistance between resistance, back electrode and the silicon chip of contact resistance, silicon chip itself of resistance, grid line and the silicon chip of grid line.The silk screen printing of electrode of solar battery silver slurry, sintering process major decision the contact resistance of positive electrode and back electrode.Therefore how forming good ohmic contact has a very big significance for the contact resistance that reduces solar cell.
Electrode is when sintering, and the glassy phase in the silver paste softens melting, makes silver along with the softening melting process of glassy phase moves to silicon face, and in process of cooling subsequently, silver carries out recrystallization at silicon chip surface, and random growth, makes it form good ohmic contact.In the existing technology, silver powder and glass powder be mechanically mixing together, and silver bag glass powder is to make silver be plated in the surface of glass powder by chemical reaction, has increased contacting of glass powder and silver powder, and contact resistance is significantly descended.
Chinese patent ZL200520069797.7 has reported that the bus electrode silver paste coats glass particle with silver, but the not open silver of this patent coats the preparation technology of glass particle.
Summary of the invention
The object of the present invention is to provide simple, the easy to operate silver paste of solar cells of a kind of processing method to wrap the preparation technology of glass powder with silver.Silver forms good ohmic contact with silicon substrate in the electrode of solar battery that the silver paste of solar cells that adopts this silver bag glass powder to prepare prepares, and can reduce its contact resistance.
A kind of silver paste of solar cells of the present invention comprises the steps: with the preparation technology of silver bag glass powder
The first step: the alligatoring of glass powder
After glass powder placed the coarsening solution ultrasonic cleaning, leave standstill to the powder sedimentation, decantation removes the upper strata coarsening solution, and remaining glass frit suspension is used washed with de-ionized water 3-5 time again, dries under room temperature, obtains the glass powder through alligatoring; Described coarsening solution is the deionized water solution of NaF and hydrochloric acid;
Second step: the activation sensitization of glass powder
After the resulting glass powder of the first step placed activation sensitizing solution ultrasonic cleaning, leave standstill to the powder sedimentation, solid-liquid separation, solid dries under the room temperature with deionized water rinsing 3-5 time, obtains the glass powder of activated sensitization; Described activation sensitizing solution is NaCl solution, SnCl
22H
2The deionized water mixed solution of O solution and hydrochloric acid;
The 3rd step: the silver parcel of glass powder
The glass powder of second step gained is added in the silver nitrate solution, in being 40～60 ℃ in temperature, after stirring and adding reductive agent reaction 3min in the silver nitrate solution simultaneously, precipitation, decantation removes upper solution, obtain the suspension of silver parcel glass powder, after washing and alcohol wash each 3 times, at room temperature dry and obtain silver and wrap glass powder.
A kind of silver paste of solar cells of the present invention wraps the preparation technology of glass powder with silver, in the alligatoring step of described glass powder, described coarsening solution is that concentration is that the NaF of 3.5～4.5g/L and concentration are the deionized water mixing solutions of 37% hydrochloric acid 35-45mL, adding 50g glass powder in every liter of described coarsening solution, is the ultrasonic 10min of ultrasonic cleaner of 100W at power.
A kind of silver paste of solar cells of the present invention is with the preparation technology of silver bag glass powder, and in the activation sensitization step of described glass powder, described activation sensitizing solution is that NaCl solution and the concentration of 300～340g/L is the SnCl of 83.33～116.67g/L by concentration
22H
2O solution, be to obtain mixed solution after 5: 3 ratio is mixed by volume, adding concentration in the described mixed solution is the hydrochloric acid of 37wt.%, addition is by every liter of interpolation of volume hydrochloric acid 62-88mL of described mixed solution, then, add deionized water to 1.25 times of described mixeding liquid volume, obtain activating sensitizing solution; Adding 50g glass powder in every liter of described activation sensitizing solution, is the ultrasonic 10min of ultrasonic cleaner of 100W at power.
A kind of silver paste of solar cells of the present invention wraps the preparation technology of glass powder with silver, in the silver parcel step of described glass powder, the mass ratio of described Silver Nitrate and glass powder is (1.5～2.0): 5, described reductive agent is ascorbic acid solution, and the addition of described reductive agent is 1 times of Silver Nitrate quality; Electric blender is adopted in described stirring, and rotating speed is 200～280RPM.
A kind of silver paste of solar cells of the present invention wraps the preparation technology of glass powder with silver, the granularity of described glass powder is 0.1-5 μ m.
A kind of silver paste of solar cells of the present invention wraps the silverskin grain graininess of glass powder less than 100nm with the preparation technology of silver bag glass powder, described silver.
The present invention is owing to adopting above-mentioned processing method, with the alligatoring of glass powder process, the sensitization activation treatment that has prepared, the then dry glass powder that obtains activating.The glass powder of activation is added respectively in silver nitrate solution, reductant solution or the end liquid, regulate the ratio of glass powder and Silver Nitrate, it is 40～60 ℃ in temperature, rotating speed is to react under 200～280RPM condition, the rear preparation-obtained nano-silver powder that reacts completely has been plated in the surface of activation glass powder, it is spent dried up washing 3 times, absolute ethanol washing 3 times, then under room temperature, dry, namely obtain silver bag glass powder.The conductive silver paste that the silver bag glass powder of the method preparation of employing patent of the present invention obtains is when carrying out sintering, glassy phase in the silver paste softens melting, make and be coated on its surperficial nanometer silverskin generation viscosity and plastic flow, make silver along with the softening melting process of glassy phase moves to silicon face, in process of cooling subsequently, silver carries out recrystallization at silicon chip surface, and random growth, make itself and silicon substrate form good ohmic contact, improved specific conductivity.This silver bag glass powder is conducive to form the supersaturation of silver in high temperature sintering, can provide enough silver at the silicon chip surface recrystallization, more effective than simple use glass powder, its reason is that the fusing point of the nano-Ag particles film that coats on the glass powder is low, diffusion when being of value to silver with the glassy phase reaction, thereby so that silver electrode and silicon substrate directly form good ohmic contact, contact resistance reduces.Present method is so that the contact area of silver and silicon substrate increases greatly, and electroconductibility is better, and contact resistance is lower, has good effect for the efficiency of conversion that improves solar cell.
In sum, processing method of the present invention is simple, easy to operate, silver forms good ohmic contact with silicon substrate in the electrode of solar battery that the silver paste of solar cells of the silver bag glass powder preparation for preparing prepares, electroconductibility is better, and can reduce its contact resistance, the efficiency of conversion of Effective Raise solar cell.Be suitable for industrial applications.
Description of drawings
Fig. 1 is the SEM figure of glass powder.
Fig. 2 is the SEM figure of preparation-obtained silver bag glass powder.
Nanometer silver has been wrapped in the surface of glass powder equably as can be seen from Figure 2, measures by transmission electron microscope, and the particle diameter of silver-colored particle is less than 100 nanometers).
Embodiment
Embodiment 1:
The roughening treatment of glass powder: take by weighing in the deionized water that 3.5gNaF is dissolved in 1000mL, add approximately 37% hydrochloric acid of 35mL concentration in consoluet NaF solution, stir, solution dilution is to 2000mL the most at last.100g glass powder is added in the coarsening solution, under the room temperature ultrasonic 10 minutes, leave standstill to the powder sedimentation, take out coarsening solution, use again the washed with de-ionized water glass powder 3 times, under room temperature, dry.
Sensitization activation treatment: the NaCl of 150g is dissolved in the 500mL deionized water, obtains solution 1; SnCl with 25g
22H
2O is dissolved in the 300mL deionized water, obtains solution 2; Solution 2 is joined in the solution 1 while stirring, obtain solution 3, and add the hydrochloric acid of 50mL37%, add at last deionized water to 1000mL, obtain sensitization, activation solution.Under the room temperature, sensitization, activation solution are poured in the 50g glass powder after the alligatoring, reaction is 10 minutes under ul-trasonic irradiation, leaves standstill afterwards, to the powder sedimentation, takes out sensitization, activation solution, with deionized water rinsing 3 times, dries under room temperature.
Glass powder after alligatoring, the sensitization activation is added in the silver nitrate solution, the mass ratio of Silver Nitrate and glass powder is 1.5: 5, and reductive agent is ascorbic acid solution, reacts completely in order to make, adopt the greatly excessive mode of reductive agent, the addition of reductive agent is 1 times of Silver Nitrate quality.Be 40 ℃ in temperature, rotating speed is that reductant solution joins in the silver nitrate solution under the electric stirring condition of 200RPM, reacts 3 minutes, and the postprecipitation that reacts completely after washing and alcohol wash each 3 times, dries under room temperature and obtains silver and wrap glass powder.
With silver powder, silver bag glass powder and doping agent and organic carrier in 80: 5: 1: the ratio of 14 (wt.%) is mixed, three rollers are ground to fineness less than 10 μ m, namely obtain the silver slurry, should be screen-printed on the monocrystalline silicon piece by the silver slurry, make monocrystaline silicon solar cell behind drying, the sintering, test its photoelectric properties, see Table 1, its electricity conversion is than not using the high 0.1 percentage point of silver bag glass powder (comparative example).
Embodiment 2:
The roughening treatment of glass powder: take by weighing in the deionized water that 4gNaF is dissolved in 1000mL, add approximately 37% hydrochloric acid of 40mL concentration in consoluet NaF solution, stir, solution dilution is to 2000mL the most at last.100g glass powder is added in the coarsening solution, under the room temperature ultrasonic 10 minutes, leave standstill to the powder sedimentation, take out coarsening solution, use again the washed with de-ionized water glass powder 3 times, under room temperature, dry.
Sensitization activation treatment: the NaCl of 160g is dissolved in the 500mL deionized water, obtains solution 1; SnCl with 30g
22H
2O is dissolved in the 300mL deionized water, obtains solution 2; Solution 2 is joined in the solution 1 while stirring, obtain solution 3, and add the hydrochloric acid of 60mL37%, add at last deionized water to 1000mL, obtain sensitization, activation solution.Under the room temperature, sensitization, activation solution are poured in the 50g glass powder after the alligatoring, reaction is 10 minutes under ul-trasonic irradiation, leaves standstill afterwards, to the powder sedimentation, takes out sensitization, activation solution, with deionized water rinsing 3 times, dries under room temperature.
Glass powder after alligatoring, the sensitization activation is added in the silver nitrate solution, the mass ratio of Silver Nitrate and glass powder is 1.75: 5, and reductive agent is ascorbic acid solution, reacts completely in order to make, adopt the greatly excessive mode of reductive agent, the addition of reductive agent is 1 times of Silver Nitrate quality.Be 50 ℃ in temperature, rotating speed is that reductant solution joins in the silver nitrate solution under the electric stirring condition of 240RPM, reacts 3 minutes, and the postprecipitation that reacts completely after washing and alcohol wash each 3 times, dries under room temperature and obtains silver and wrap glass powder.
With silver powder, silver bag glass powder and doping agent and organic carrier in 80: 5: 1: the ratio of 14 (wt.%) is mixed, three rollers are ground to fineness less than 10 μ m, namely obtain the silver slurry, should be screen-printed on the monocrystalline silicon piece by the silver slurry, make monocrystaline silicon solar cell behind drying, the sintering, test its photoelectric properties, see Table 1, its electricity conversion is than not using the high 0.3 percentage point of silver bag glass powder (comparative example).
Embodiment 3:
The roughening treatment of glass powder: take by weighing in the deionized water that 4.5gNaF is dissolved in 1000mL, add approximately 37% hydrochloric acid of 45mL concentration in consoluet NaF solution, stir, solution dilution is to 2000mL the most at last.100g glass powder is added in the coarsening solution, under the room temperature ultrasonic 10 minutes, leave standstill to the powder sedimentation, take out coarsening solution, use again the washed with de-ionized water glass powder 3 times, under room temperature, dry.
Sensitization activation treatment: the NaCl of 170g is dissolved in the 500mL deionized water, obtains solution 1; SnCl with 35g
22H
2O is dissolved in the 300mL deionized water, obtains solution 2; Solution 2 is joined in the solution 1 while stirring, obtain solution 3, and add the hydrochloric acid of 70mL37%, add at last deionized water to 1000mL, obtain sensitization, activation solution.Under the room temperature, sensitization, activation solution are poured in the 50g glass powder after the alligatoring, reaction is 10 minutes under ul-trasonic irradiation, leaves standstill afterwards, to the powder sedimentation, takes out sensitization, activation solution, with deionized water rinsing 3 times, dries under room temperature.
Glass powder after alligatoring, the sensitization activation is added in the silver nitrate solution, the mass ratio of Silver Nitrate and glass powder is 2: 5, and reductive agent is ascorbic acid solution, reacts completely in order to make, adopt the greatly excessive mode of reductive agent, the addition of reductive agent is 1 times of Silver Nitrate quality.Be 60 ℃ in temperature, rotating speed is that reductant solution joins in the silver nitrate solution under the electric stirring condition of 280RPM, reacts 3 minutes, and the postprecipitation that reacts completely after washing and alcohol wash each 3 times, dries under room temperature and obtains silver and wrap glass powder.
With silver powder, silver bag glass powder and doping agent and organic carrier in 80: 5: 1: the ratio of 14 (wt.%) is mixed, three rollers are ground to fineness less than 10 μ m, namely obtain the silver slurry, should be screen-printed on the monocrystalline silicon piece by the silver slurry, make monocrystaline silicon solar cell behind drying, the sintering, test its photoelectric properties, see Table 1, its electricity conversion is than not using the high 0.2 percentage point of silver bag glass powder (comparative example).
Comparative example:
With silver powder, glass powder and doping agent and organic carrier in 80: 5: 1: the ratio of 14 (wt.%) is mixed, three rollers are ground to fineness less than 10 μ m, namely obtain the silver slurry, should be screen-printed on the monocrystalline silicon piece by the silver slurry, make monocrystaline silicon solar cell behind drying, the sintering, test its photoelectric properties, see Table 1, its electricity conversion is than using silver-colored low 0.1～0.3 percentage point of wrapping glass powder (embodiment 1～3).
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example | |
| V oc(V) | 0.630427 | 0.630245 | 0.628504 | 0.628718 |
| I sc(A) | 5.852708 | 5.748002 | 5.757717 | 5.796954 |
| P mp(W) | 2.848079 | 2.829119 | 2.804439 | 2.788744 |
| V mp(V) | 0.51926 | 0.523027 | 0.518792 | 0.515601 |
| I mp(A) | 5.484879 | 5.409122 | 5.405708 | 5.408727 |
| FF(％) | 77.18986 | 78.09532 | 77.49753 | 76.51612 |
| R s(Ω) | 0.008858 | 0.008454 | 0.008869 | 0.009375 |
| R sh(Ω) | 12.83855 | 127.53 | 38.81212 | 58.17953 |
| Eff(％) | 18.39844 | 18.27597 | 18.11653 | 18.01514 |
Table 1 explanation: the P of three embodiment batteries
Mp, V
Mp, FF and Eff be than the height of comparative example, the R of embodiment
sAll lower than the comparative example, the V of embodiment
Oc, I
MpAnd R
ShCompare with comparative example, it is low that some height have.For the crystal silicon solar energy battery of an excellent property, in general, P
Mp, V
Mp, FF, Eff, V
Oc, I
MpAnd R
ShAll be more high better, R
sMore low better, in actual applications, some batteries most effective, but certain several parameter is higher or on the low side, but the over-all properties of final battery is by the Eff evaluation, in general, Eff is higher, and the performance of battery is more excellent, and the over-all properties of experimental example 1 battery is best in the table 1.
Claims (6)
1. silver paste of solar cells wraps glass powder with silver a preparation technology comprises the steps:
The first step: the alligatoring of glass powder
After glass powder placed the coarsening solution ultrasonic cleaning, leave standstill to the powder sedimentation, decantation removes the upper strata coarsening solution, and remaining glass frit suspension is used washed with de-ionized water 3-5 time again, dries under room temperature, obtains the glass powder through alligatoring; Described coarsening solution is the deionized water solution of NaF and hydrochloric acid;
Second step: the activation sensitization of glass powder
After the resulting glass powder of the first step placed activation sensitizing solution ultrasonic cleaning, leave standstill to the powder sedimentation, solid-liquid separation, solid dries under the room temperature with deionized water rinsing 3-5 time, obtains the glass powder of activated sensitization; Described activation sensitizing solution is NaCl solution, SnCl
22H
2The deionized water mixed solution of O solution and hydrochloric acid;
The 3rd step: the silver parcel of glass powder
The glass powder of second step gained is added in the silver nitrate solution, in being 40～60 ℃ in temperature, after stirring and adding reductive agent reaction 3min in the silver nitrate solution simultaneously, precipitation, decantation removes upper solution, obtain the suspension of silver parcel glass powder, after washing and alcohol wash each 3 times, at room temperature dry and obtain silver and wrap glass powder.
2. a kind of silver paste of solar cells according to claim 1 wraps the preparation technology of glass powder with silver, it is characterized in that: in the alligatoring step of described glass powder, described coarsening solution is that concentration is that the NaF of 3.5～4.5g/L and concentration are the deionized water mixing solutions of 37% hydrochloric acid 35-45mL, adding 50g glass powder in every liter of described coarsening solution, is the ultrasonic 10min of ultrasonic cleaner of 100W at power.
3. a kind of silver paste of solar cells according to claim 2 wraps the preparation technology of glass powder with silver, it is characterized in that: in the activation sensitization step of described glass powder, described activation sensitizing solution is that NaCl solution and the concentration of 300～340g/L is the SnCl of 83.33～116.67g/L by concentration
22H
2O solution, be to obtain mixed solution after 5: 3 ratio is mixed by volume, adding concentration in the described mixed solution is the hydrochloric acid of 37wt.%, addition is by every liter of interpolation of volume hydrochloric acid 62-88mL of described mixed solution, then, add deionized water to 1.25 times of described mixeding liquid volume, obtain activating sensitizing solution; Adding 50g glass powder in every liter of described activation sensitizing solution, is the ultrasonic 10min of ultrasonic cleaner of 100W at power.
4. a kind of silver paste of solar cells according to claim 3 wraps the preparation technology of glass powder with silver, it is characterized in that: in the silver parcel step of described glass powder, the mass ratio of described Silver Nitrate and glass powder is (1.5～2.0): 5, described reductive agent is ascorbic acid solution, and the addition of described reductive agent is 1 times of Silver Nitrate quality; Electric blender is adopted in described stirring, and rotating speed is 200～280RPM.
5. a kind of silver paste of solar cells according to claim 4 wraps the preparation technology of glass powder with silver, and it is characterized in that: the granularity of described glass powder is 0.1-5 μ m.
6. the described a kind of silver paste of solar cells of any one uses silver to wrap the preparation technology of glass powder according to claim 1-5, it is characterized in that: the silverskin grain graininess of described silver bag glass powder is less than 100nm.
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| CN105321594B (en) * | 2015-02-26 | 2017-04-26 | 深圳市春仰科技有限公司 | Positive silver paste of silicon solar cell and preparation method of positive silver paste |
| CN107324664A (en) * | 2017-06-16 | 2017-11-07 | 北京市合众创能光电技术有限公司 | A kind of method of modifying of solar cell conductive silver paste glass dust |
| CN107742658A (en) * | 2017-11-10 | 2018-02-27 | 扬州鑫晶光伏科技有限公司 | A solar photovoltaic cell |
| CN107742546A (en) * | 2017-11-10 | 2018-02-27 | 扬州鑫晶光伏科技有限公司 | Environment-friendly silver paste for front electrode of solar photovoltaic cell and preparation method thereof |
| CN109183010B (en) * | 2018-11-01 | 2020-11-10 | 中钢集团马鞍山矿院新材料科技有限公司 | Method for roughening surface of hollow glass bead and plating nickel |
| CN110698071B (en) * | 2019-09-30 | 2022-06-21 | 湖南诺尔得材料科技有限公司 | Preparation method of composite glass powder and conductive silver paste |
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| CN114530508B (en) * | 2020-11-02 | 2024-10-18 | 苏州阿特斯阳光电力科技有限公司 | PERC cells and photovoltaic modules |
| CN114447123B (en) * | 2020-11-02 | 2024-05-14 | 苏州阿特斯阳光电力科技有限公司 | Heterojunction solar cell and photovoltaic module |
| CN116618674B (en) * | 2023-05-11 | 2024-02-02 | 湖北银科新材料股份有限公司 | Preparation method of surface high-activity modified silver powder |
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