CN110033875A - A kind of preparation method of crystal silicon photovoltaic cell front electrode silver slurry - Google Patents
A kind of preparation method of crystal silicon photovoltaic cell front electrode silver slurry Download PDFInfo
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- CN110033875A CN110033875A CN201910405106.2A CN201910405106A CN110033875A CN 110033875 A CN110033875 A CN 110033875A CN 201910405106 A CN201910405106 A CN 201910405106A CN 110033875 A CN110033875 A CN 110033875A
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- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 68
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 44
- 239000004332 silver Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000002002 slurry Substances 0.000 title claims abstract description 19
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 17
- 239000010703 silicon Substances 0.000 title claims abstract description 17
- 239000013078 crystal Substances 0.000 title claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000011521 glass Substances 0.000 claims abstract description 23
- 239000002270 dispersing agent Substances 0.000 claims abstract description 22
- 235000019353 potassium silicate Nutrition 0.000 claims abstract description 16
- 239000004111 Potassium silicate Substances 0.000 claims abstract description 15
- 229910052913 potassium silicate Inorganic materials 0.000 claims abstract description 15
- NNHHDJVEYQHLHG-UHFFFAOYSA-N potassium silicate Chemical compound [K+].[K+].[O-][Si]([O-])=O NNHHDJVEYQHLHG-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 14
- 229910021485 fumed silica Inorganic materials 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 9
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 4
- 235000019795 sodium metasilicate Nutrition 0.000 claims abstract description 4
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 13
- 239000000377 silicon dioxide Substances 0.000 claims description 8
- 238000000498 ball milling Methods 0.000 claims description 7
- 239000002131 composite material Substances 0.000 claims description 7
- 239000000203 mixture Substances 0.000 claims description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 230000001476 alcoholic effect Effects 0.000 claims description 2
- 229910052681 coesite Inorganic materials 0.000 claims description 2
- 229910052906 cristobalite Inorganic materials 0.000 claims description 2
- 229910052682 stishovite Inorganic materials 0.000 claims description 2
- 229910052905 tridymite Inorganic materials 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 8
- 238000007639 printing Methods 0.000 abstract description 7
- 238000005245 sintering Methods 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 5
- 239000006185 dispersion Substances 0.000 abstract description 4
- 239000012153 distilled water Substances 0.000 description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 230000009974 thixotropic effect Effects 0.000 description 7
- WTDHULULXKLSOZ-UHFFFAOYSA-N Hydroxylamine hydrochloride Chemical compound Cl.ON WTDHULULXKLSOZ-UHFFFAOYSA-N 0.000 description 6
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 6
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 description 6
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 5
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 5
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000010008 shearing Methods 0.000 description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000000908 ammonium hydroxide Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000010946 fine silver Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 229910001961 silver nitrate Inorganic materials 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 description 2
- KDYFGRWQOYBRFD-UHFFFAOYSA-N succinic acid Chemical compound OC(=O)CCC(O)=O KDYFGRWQOYBRFD-UHFFFAOYSA-N 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 description 1
- 229910001950 potassium oxide Inorganic materials 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000007613 slurry method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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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
- H01B1/14—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
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Sustainable Energy (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Electromagnetism (AREA)
- General Physics & Mathematics (AREA)
- Computer Hardware Design (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Power Engineering (AREA)
- Glass Compositions (AREA)
- Photovoltaic Devices (AREA)
- Conductive Materials (AREA)
Abstract
The present invention relates to silicon systems photovoltaic cell preparation technical fields, and disclose a kind of preparation method of crystal silicon photovoltaic cell front electrode silver slurry, average grain diameter≤150um silver powder and the glass powder of uniform dispersion bonding are added in inorganic carrier solvent high mode potassium silicate solution, under the collective effect of inorganic dispersant sodium metasilicate and inorganic anti-settling agent fumed silica, silver powder is in homogeneously dispersed state in the slurry, prepares crystal silicon photovoltaic cell front electrode silver slurry.The present invention solves current silicon systems battery front side electrode silver paste, and during silver powder is prepared into silver paste, used organic dispersing agent causes printing striped crack in sintering process emergent gas, not can guarantee battery front side silver electrode and stablizes conductive technical problem.
Description
Technical field
The present invention relates to silicon systems photovoltaic cell preparation technical field, specially a kind of crystal silicon photovoltaic cell front electrode silver
The preparation method of slurry.
Background technique
Further increasing the photoelectric conversion efficiency of battery and reducing cost of manufacture is that solar battery manufacturing industry is pursued forever
Permanent target, for silicon systems solar battery, if it is more difficult for thinking further to improve efficiency.Therefore, the weight researched and developed from now on
On the one hand point is to continue with develops novel battery material, on the other hand should concentrate on how reducing in cost.High-efficiency photovoltaic is too
Positive energy battery request front silver electrode " thin grid dense planting ", will obtain the front electrode that grid line is thin, pattern is smooth, to conductive silver
The requirement of slurry is that easily net, good leveling property, depth-width ratio are big excessively, i.e., has particular/special requirement to the rheologic behavio(u)r of slurry.
For the front electrode silver slurry used for solar batteries of silk-screen printing, ingredient specifically includes that silver powder conductive phase, organic
Carrier solvent, a small amount of glass powder Binder Phase.For the silver powder of solar cell front side silver paste, it is big generally to reach micron
Small or sub-micron partial size.During silver powder is prepared into silver paste, surfactant is a very important ginseng
Number can be effectively improved the dispersibility, size distribution and tap density of silver powder by adding suitable dispersing agent.At present about
Surfactant selection is mainly organic dispersing agent, wherein most representational is polyvinylpyrrolidone (PVP) dispersing agent,
Although the above-mentioned silver paste function admirable prepared using PVP dispersing agent, above-mentioned PVP dispersing agent are belonged to backbone, starched
There are the expansion issues of sintering process in the application of material, and moreover, solar cell front side silver paste will be by 700 DEG C or more
High temperature sintering, due to containing many carbon atoms in the PVP dispersing agent of backbone, during the sintering process, carbon atom burning becomes
Carbon dioxide evolution causes printing striped crack, to influence the electrical property of solar cell front side silver electrode.
The present invention provides a kind of preparation method of crystal silicon photovoltaic cell front electrode silver slurry, it is intended to solve current silicon systems electricity
Pond front electrode silver slurry, during silver powder is prepared into silver paste, used organic dispersing agent escapes gas in sintering process
Body causes printing striped crack, not can guarantee battery front side silver electrode and stablizes conductive technical problem.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of preparation sides of crystal silicon photovoltaic cell front electrode silver slurry
Method solves current silicon systems battery front side electrode silver paste, during silver powder is prepared into silver paste, used organic dispersion
Agent causes printing striped crack in sintering process emergent gas, not can guarantee the stable conductive technology of battery front side silver electrode and asks
Topic.
(2) technical solution
To achieve the above object, the invention provides the following technical scheme:
A kind of preparation method of crystal silicon photovoltaic cell front electrode silver slurry, comprising the following steps:
(1) 90~120 parts of average grain diameter≤150um silver powder are prepared；
(2) 10~15 parts are weighed by PbO, SiO2、TiO2、B2O3, 10%wtMgO composition glass powder, ultrasonic disperse is in nothing
In alcoholic solvent, preparation obtains glass dispersible liquid；
(3) 15~25 parts of high mode potassium silicate solutions are added in super mixer, are stirring for 300~500rpm in revolving speed
It mixes under state, 1~3 part of dispersing agent and 2~3 portions of anti-settling agents is first added, be slow added into the silver powder prepared in step (1), switch to
600~800rpm stirs 2~3h；
It, will the middle glass prepared point of step (2) with the rate of 1mL/s in the case where revolving speed is the stirring of 300~500rpm
Dispersion liquid is added in super mixer, later, is switched to 600~800rpm and is stirred 1~3h；
(4) composite mortar prepared in step (3) is placed in ball grinder and carries out ball milling, sieved with 100 mesh sieve, silver is prepared
Slurry.
Preferably, in the step (2), glass powder is by average grain diameter≤2.6um 30%wtPbO, 20%wtSiO2、
25%wtTiO2, 15%wtB2O3, 10%wtMgO composition.
Preferably, in the step (3), dispersing agent is sodium metasilicate, anti-settling agent is fumed silica.
Preferably, in the step (4), composite mortar is in N2Protection is lower to carry out ball milling.
(3) beneficial technical effect
Compared with prior art, the present invention has following beneficial technical effect:
Average grain diameter≤150um silver powder and the glass powder of uniform dispersion bonding are added to inorganic carrier solvent Gao Mo
In number potassium silicate solution, under the collective effect of inorganic dispersant sodium metasilicate and inorganic anti-settling agent fumed silica, silver powder exists
It is in homogeneously dispersed state in slurry, prepares crystal silicon photovoltaic cell front electrode silver slurry；
Above-mentioned crystal silicon photovoltaic cell front electrode silver slurry, during silver powder is prepared into silver paste, due to use
Carrier solvent, dispersing agent and anti-settling agent are inorganic high-temperature resistant component, without using organic dispersing agent, so after silver paste printing
During sintering, will not emergent gas, cause printing striped crack, so as to be effectively ensured battery front side silver electrode stablize
Conductive technical effect；
The thixotropic index for the silver paste that the present invention prepares is 2.72~2.80, shows that silver paste viscosity when not stressing is larger,
It is reduced rapidly by viscosity when shearing force, shows pseudoplastic behavior, silver paste between mesh from discharging and fast quick-recovery is to initial again after printing
Structure is not in sprawl and collapse, therefore the silver paste prepared of the present invention has and is easy to print the good technology of net, continuity
Advantage.
Specific embodiment
The high mode potassium silicate solution used in following embodiment is all made of following methods preparation.
The raw material for preparing high mode potassium silicate solution include: potassium silicate solution, Qingdao water glass plant；Silica solution, Jiangyin
Chemical Co., Ltd., League of Nations；Methyltrimethoxysilane, chemical pure, Solution on Chemical Reagents in Shanghai purchasing and supply station；Wherein, potassium silicate is molten
The fundamental property of liquid is shown in Table 1, and the fundamental property of silica solution is shown in Table 2；
The fundamental property of 1 potassium silicate solution of table
| Specification | Potassium oxide % | Silica % | Modulus (M) | Viscosity (20 DEG C) Pas |
| QPY405-1 | ≥11.5 | ≥25 | 3.15~3.3 | ≤0.6 |
The fundamental property of 2 silica solution of table
The preparation method of high mode potassium silicate solution is the following steps are included: pouring into 100g potassium silicate solution equipped with high-speed stirring
In the reactor for mixing device and heating device, it is slowly added into 15g silica solution under stiring, after dripping silica solution, system is heated up
To 50 DEG C, then 6g methyltrimethoxysilane is added dropwise into reactor, adding distilled water in the process makes the pH value of system
10, after dripping silane, 2.0h is stirred at 3500r/min to get high mode potassium silicate solution is arrived.
Embodiment one:
(1) it takes 150g silver nitrate to be dissolved in distilled water, the ammonium hydroxide that 100mL mass fraction is 10% is added, is settled to 2L,
Constant temperature is kept at 40 DEG C of temperature, preparation obtains solution A；1g sodium hydroxide is taken to be dissolved in 2L distilled water, preparation obtains solution
B；
(2) solution B is added in the reactor equipped with agitating device and heating device, keeps permanent at 40 DEG C of temperature
Temperature is first added the hydroxylamine hydrochloride solution that 200g mass fraction is 10%, adds 0.5g amber in the case where revolving speed is the stirring of 120rpm
Amber acid switchs to 300rpm stirring 1h, while keeping constant temperature at 40 DEG C of temperature；
(3) reactor in step (2) keeps constant temperature at 40 DEG C of temperature, and in the case where revolving speed is the stirring of 120rpm, will
Solution A is added in reactor with the rate of 5mL/s, after solution A is added dropwise, is switched to 300rpm and is stirred to react 1h, later, together
When keep constant temperature at 40 DEG C of temperature；
After reaction, it adopts until being washed with distilled water to conductivity as 10us/cm, gained super fine silver powder is placed on very
In empty drying box, 1h is kept the temperature under temperature 60 C, grinding sieves with 100 mesh sieve, and average grain diameter≤150um silver powder is prepared；
(4) 10g average grain diameter≤2.6um glass powder is weighed, ultrasonic disperse joined 1g silicate dispersant and 2g
In the 100mL anhydrous ethanol solvent of fumed silica anti-settling agent, preparation obtains glass dispersible liquid；Wherein, glass powder is by 30%
WtPbO, 20%wtSiO2, 25%wtTiO2, 15%wtB2O3, 10%wtMgO composition；
(5) 15g high mode potassium silicate solution is added in super mixer, in the case where revolving speed is the stirring of 300rpm,
1g silicate dispersant and 2g fumed silica anti-settling agent is first added, is slow added into the 90g silver powder prepared in step (3),
Switch to 600rpm stirring 2h；
In the case where revolving speed is the stirring of 300rpm, the glass dispersible liquid prepared in step (4) is added with the rate of 1mL/s
Enter into super mixer, later, switchs to 600rpm stirring 1h；
(6) composite mortar prepared in step (5) is placed in ball grinder, in N2Under protection, ball milling 4h is sieved with 100 mesh sieve,
Silver paste is prepared；
(7) testing above-mentioned silver paste in shear rate is 10s-1Under viscosity be 56.3Pas, shear rate be 100s-1
Under viscosity be 20.1Pas, thixotropic index 2.80.
Embodiment two:
(1) it takes 180g silver nitrate to be dissolved in distilled water, the ammonium hydroxide that 100mL mass fraction is 10% is added, is settled to 2L,
Constant temperature is kept under temperature 50 C, preparation obtains solution A；1.5g sodium hydroxide is taken to be dissolved in 2L distilled water, preparation obtains molten
Liquid B；
(2) solution B is added in the reactor equipped with agitating device and heating device, keeps permanent under temperature 50 C
Temperature is first added the hydroxylamine hydrochloride solution that 220g mass fraction is 10%, adds 0.8g amber in the case where revolving speed is the stirring of 200rpm
Amber acid switchs to 400rpm stirring 2h, while keeping constant temperature under temperature 50 C；
(3) reactor in step (2) keeps constant temperature under temperature 50 C, and in the case where revolving speed is the stirring of 200rpm, will
Solution A is added in reactor with the rate of 5mL/s, after solution A is added dropwise, is switched to 400rpm and is stirred to react 2h, later, together
When keep constant temperature under temperature 50 C；
After reaction, it adopts until being washed with distilled water to conductivity as 30us/cm, gained super fine silver powder is placed on very
In empty drying box, 2h is kept the temperature under temperature 50 C, grinding sieves with 100 mesh sieve, and average grain diameter≤150um silver powder is prepared；
(4) weigh 12g average grain diameter≤2.6um glass powder, ultrasonic disperse joined 2g silicate dispersant and
In the 100mL anhydrous ethanol solvent of 2.5g fumed silica anti-settling agent, preparation obtains glass dispersible liquid；Wherein, glass powder by
30%wtPbO, 20%wtSiO2, 25%wtTiO2, 15%wtB2O3, 10%wtMgO composition；
(5) 20g high mode potassium silicate solution is added in super mixer, in the case where revolving speed is the stirring of 400rpm,
2g silicate dispersant and 2.5g fumed silica anti-settling agent is first added, is slow added into the 108g silver prepared in step (3)
Powder switchs to 700rpm stirring 2.5h；
In the case where revolving speed is the stirring of 400rpm, the glass dispersible liquid prepared in step (4) is added with the rate of 1mL/s
Enter into super mixer, later, switchs to 700rpm stirring 2h；
(6) composite mortar prepared in step (5) is placed in ball grinder, in N2Under protection, ball milling 5h is sieved with 100 mesh sieve,
Silver paste is prepared；
(7) testing above-mentioned silver paste in shear rate is 10s-1Under viscosity be 55.7Pas, shear rate be 100s-1
Under viscosity be 20.5Pas, thixotropic index 2.72.
Embodiment three:
(1) it takes 200g silver nitrate to be dissolved in distilled water, the ammonium hydroxide that 100mL mass fraction is 10% is added, is settled to 2L,
Constant temperature is kept under temperature 60 C, preparation obtains solution A；1.5g sodium hydroxide is taken to be dissolved in 2L distilled water, preparation obtains molten
Liquid B；
(2) solution B is added in the reactor equipped with agitating device and heating device, keeps permanent under temperature 60 C
Temperature is first added the hydroxylamine hydrochloride solution that 260g mass fraction is 10%, adds 1g amber in the case where revolving speed is the stirring of 300rpm
Acid switchs to 500rpm stirring 3h, while keeping constant temperature under temperature 60 C；
(3) reactor in step (2) keeps constant temperature under temperature 60 C, and in the case where revolving speed is the stirring of 300rpm, will
Solution A is added in reactor with the rate of 5mL/s, after solution A is added dropwise, is switched to 500rpm and is stirred to react 3h, later, together
When keep constant temperature under temperature 60 C；
After reaction, it adopts until being washed with distilled water to conductivity as 50us/cm, gained super fine silver powder is placed on very
In empty drying box, 3h is kept the temperature under temperature 60 C, grinding sieves with 100 mesh sieve, and average grain diameter≤150um silver powder is prepared；
(4) 15g average grain diameter≤2.6um glass powder is weighed, ultrasonic disperse joined 3g silicate dispersant and 3g
In the 100mL anhydrous ethanol solvent of fumed silica anti-settling agent, preparation obtains glass dispersible liquid；Wherein, glass powder is by 30%
WtPbO, 20%wtSiO2, 25%wtTiO2, 15%wtB2O3, 10%wtMgO composition；
(5) 25g high mode potassium silicate solution is added in super mixer, in the case where revolving speed is the stirring of 500rpm,
3g silicate dispersant and 3g fumed silica anti-settling agent is first added, is slow added into the 120g silver powder prepared in step (3),
Switch to 800rpm stirring 3h；
In the case where revolving speed is the stirring of 500rpm, the glass dispersible liquid prepared in step (4) is added with the rate of 1mL/s
Enter into super mixer, later, switchs to 800rpm stirring 3h；
(6) composite mortar prepared in step (5) is placed in ball grinder, in N2Under protection, ball milling 6h is sieved with 100 mesh sieve,
Silver paste is prepared；
(7) testing above-mentioned silver paste in shear rate is 10s-1Under viscosity be 55.1Pas, shear rate be 100s-1
Under viscosity be 19.9Pas, thixotropic index 2.77.
Wherein, it is now widely used it is main to the parameter of slurry rheological property characterization there are two: one is that specific shearing is fast
Viscosity under rate, common shear rate are 10s-1Under viscosity, the other is thixotropic index, also referred to as thixotropic coefficient, reflection slurry
Expect the thixotropy under shearing force, usual shearing rate is in 10s in practical application-1Under viscosity and 100s-1Under viscosity
Ratio makees thixotropic coefficient value.
Claims (4)
1. a kind of preparation method of crystal silicon photovoltaic cell front electrode silver slurry, which comprises the following steps:
(1) 90~120 parts of average grain diameter≤150um silver powder are prepared；
(2) 10~15 parts are weighed by PbO, SiO2、TiO2、B2O3, 10%wtMgO composition glass powder, ultrasonic disperse is in anhydrous second
In alcoholic solvent, preparation obtains glass dispersible liquid；
(3) 15~25 parts of high mode potassium silicate solutions are added in super mixer, in the stirring shape that revolving speed is 300~500rpm
Under state, 1~3 part of dispersing agent and 2~3 portions of anti-settling agents are first added, are slow added into the silver powder prepared in step (1), switch to 600~
800rpm stirs 2~3h；
It, will the middle glass dispersible liquid prepared of step (2) with the rate of 1mL/s in the case where revolving speed is the stirring of 300~500rpm
It is added in super mixer, later, switchs to 600~800rpm and stir 1~3h；
(4) composite mortar prepared in step (3) is placed in ball grinder and carries out ball milling, sieved with 100 mesh sieve, silver paste is prepared.
2. preparation method according to claim 1, which is characterized in that in the step (2), glass powder by average grain diameter≤
30%wtPbO, 20%wtSiO of 2.6um2, 25%wtTiO2, 15%wtB2O3, 10%wtMgO composition.
3. preparation method according to claim 1, which is characterized in that in the step (3), dispersing agent is sodium metasilicate, prevents
Heavy agent is fumed silica.
4. preparation method according to claim 1, which is characterized in that in the step (4), composite mortar is in N2Under protection
Carry out ball milling.
Priority Applications (1)
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| CN110449572A (en) * | 2019-08-08 | 2019-11-15 | 湖南诺尔得材料科技有限公司 | The preparation method of the functional silver powder of electric slurry |
| CN111210923A (en) * | 2020-03-19 | 2020-05-29 | 德阳烯碳科技有限公司 | Conductive silver paste and preparation process thereof |
| CN112447330A (en) * | 2020-11-16 | 2021-03-05 | 无锡帝科电子材料股份有限公司 | Preparation method of high-performance silver ink |
| CN113299422A (en) * | 2021-05-07 | 2021-08-24 | 江西师范大学 | Crystalline silicon solar cell front silver paste and preparation method thereof |
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