CN102351403B - Method for preparing ultrafine glass powder used for solar battery slurry - Google Patents
Method for preparing ultrafine glass powder used for solar battery slurry Download PDFInfo
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- CN102351403B CN102351403B CN 201110200826 CN201110200826A CN102351403B CN 102351403 B CN102351403 B CN 102351403B CN 201110200826 CN201110200826 CN 201110200826 CN 201110200826 A CN201110200826 A CN 201110200826A CN 102351403 B CN102351403 B CN 102351403B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/02—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture in electric furnaces, e.g. by dielectric heating
- C03B5/021—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture in electric furnaces, e.g. by dielectric heating by induction heating
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
- C03B19/1005—Forming solid beads
- C03B19/1045—Forming solid beads by bringing hot glass in contact with a liquid, e.g. shattering
Abstract
The invention provides a method for preparing ultrafine glass powder used for solar battery slurry. The method comprises the following steps: placing of a burden and a mixture in a corundum crucible with a graphite capsule, heating and fusing step by step in an induction furnace, water quenching and fragmenting, drying, sieving and packaging. According to the invention, the graphite capsule is taken as a heat-generating body which solves the defects of non-conducting and unheating of glass materials in the induction furnace. The employed induction heating mode has fast heating speed, and is capable of minimizing the volatilization of glass component during the melting process, minimizing the environmental pollution, ensuring the small difference between the prepared glass powder and the designed component, and effectively ensuring the stability of the glass powder component; the production cost is low and the production efficiency is high, the component of the finished product enables a basic conformity with the design. The used step heating mode ensures the basically synchronous heating of the graphite capsule, the corundum crucible and oxide raw materials for melting glass, solves the problem that the temperature difference between internal and external of the corundum crucible caused by heat transmission delay is excessive so that the excessive thermal stress leads to breakage of the corundum crucible; and the method is suitable for industrial production.
Description
Technical field
Patent of the present invention relates to the preparation technology that a kind of solar cell size is used palladium powder.Belong to the solar cell preparing technical field.
Background technology
Glass powder can be applicable to a lot of fields according to its composition difference, for example: can add in the paint, increase hardness, the toughness of paint, improve the anti scuffing performance of paint film, have photoextinction, improve the weathering resistance of paint film; Can add in the slurry, have suitable temperature of fusion and sealing temperature, good thermotolerance and chemical stability, high physical strength and good sealing-in resistance to air loss.
Glass powder also can be applicable to the preparation of solar cell size.Glass powder liquefies when Fast Sintering, plays cohesive action between silver powder and silicon substrate, plays the effect that penetrates antireflective coating simultaneously, makes between silver powder and the silicon substrate and forms good Ohmic contact.The composition of glass powder, content, size and softening temperature can directly influence contact resistance, penetrate the conductivity of antireflective coating ability, electrode and the sticking power between electrode and the substrate etc., thereby influence electricity conversion and the work-ing life of solar cell.Present stage, solar cell size mainly is divided into flint glass powder and lead-free glass powder with palladium powder.Flint glass at softening temperature, thermal expansivity, penetrate antireflective coating and form and have a clear superiority in aspect the ohmic contact.Crown glass is mainly the bismuthate system, utilizes bismuth element to substitute the effect of lead element in glass, reduces to the pollution of environment with to the harm of human body, be solar cell size with the main developing direction of palladium powder, now progressively use.
At present, the preparation technology commonly used of glass powder is: mixed compound is put into crucible, put into furnace temperature then and be 1200 ℃～1400 ℃ High Temperature Furnaces Heating Apparatus, glass metal after the fusing is poured in the cold water, granular glass, abrading-ball and ball-milling medium are put into the ball mill ball milling, glass powder behind the ball milling is sieved pack.Common process can satisfy the requirement of most of glass powder preparations, but has following weak point:
(1) High Temperature Furnaces Heating Apparatus is long heat-up time, and being warming up to general glass melting temperature needs about 6 hours, makes that glass powder production efficiency is low, and production cost increases;
(2) compound is if be in the hot environment for a long time, and composition wherein volatilizees easily, causes glass powder product and formulating of recipe not to be inconsistent.If contain lead in the glass powder, when founding these glass, a large amount of the evaporateing in the air of plumbous meeting cause serious harm to environment and human body.
Summary of the invention
The purpose of patent of the present invention is to overcome conventional preparation technology's above-mentioned defective, provide a kind of faster, the low-cost high-efficiency glass powder preparation technology of You Huaing more guarantees the stability of glass powder composition, the composition of finished product conforms to design substantially, reduces the pollution to environment.
A kind of solar cell size of the present invention comprises the steps: with the preparation technology of palladium powder
The first step: batching
Component prescription by design takes by weighing each raw material, mixes, and obtains compound;
Second step: heat fused
The first step gained compound is put into the corundum crucible that has the graphite jacket, at the induction furnace internal heating to temperature of fusion 1200-1700 ℃;
The 3rd step: broken after the shrend
Pour the glass metal that second step obtained in deionized water shrend; Ball milling is 2.5～3.0 microns to D50 then, and D90 is 4～5 microns; Dry, sieve and pack.
A kind of solar cell size of the present invention adopts the graphite jacket with the preparation technology of palladium powder, described corundum crucible, and graphite is wrapped in heating in the induction furnace and heat is reached compound in the corundum crucible, makes its fusing.
A kind of solar cell size of the present invention preparation technology of palladium powder, described heat fused divides five stages to finish, and first section, mixture temperature rises to 500～600 ℃ by room temperature, and temperature rise rate is 40-50 ℃/minute; Second section, mixture temperature rises to 800～850 ℃, and temperature rise rate is 30-40 ℃/minute; The 3rd section, mixture temperature rises to 1000～1050 ℃, and temperature rise rate is 20-30 ℃/minute; The 4th section, mixture temperature rises to 1100～1150 ℃, and temperature rise rate is 15-20 ℃/minute; The 5th section, mixture temperature rises to the glass smelting temperature, and temperature rise rate is 10-15 ℃/minute.
A kind of solar cell size of the present invention preparation technology of palladium powder, described ball milling adopts wet ball-milling, ball-milling medium is alcohol, material, abrading-ball and alcohol are according to 0.5～1.2: 0.8～1.5: 1～2 ratio is put into ball mill and is carried out ball milling, ball-milling technology is: 10～25 hours ball milling time, rotating speed is 280～350 rev/mins.
The present invention is owing to adopt graphite jacket corundum crucible in the induction furnace heat fused, on the one hand, utilize graphite as heating element, be close to the corundum crucible that compound is housed, effectively heat is conducted to compound, compound is founded into glass, overcome the oxide raw material of fusion cast glass and corundum crucible and under normal condition, be isolator, defective that can not the self-heating fusing in induction furnace; On the other hand, adopt the induction furnace heating, can reach the glass melting temperature of glass within a short period of time, it is long to overcome the prior art melting time, the unsettled defective of glass powder composition.Particularly, the present invention adopts the mode of substep heating, the oxide raw material basic synchronization that can guarantee graphite jacket, corundum crucible, fusion cast glass heats up, solved that to delay the corundum crucible internal-external temperature difference that causes excessive owing to the heat transmission, suffered thermal stresses is excessive, the problem that corundum crucible is broken; Because heat conducts to corundum crucible by the graphite jacket, conducts to the process that compound is heated it and melts again, needs the regular hour.In this course, if heat-up rate is too fast, the heat-up rate of graphite jacket causes the corundum crucible internal-external temperature difference excessive obviously greater than the heat-up rate of compound in the corundum crucible, and suffered thermal stresses is excessive, and corundum crucible is broken.If rate of heating is slow excessively, can cause the melting time of compound long, can result from the same detrimentally affect of common process.So need make suitable technology, the whole heat-processed of strict control obtains high-quality glass powder.
Find by a large amount of practices how many corundum crucible size of heating process and graphite jacket and amounts of the compound of adorning have very big relation.Long with the whole process of founding for avoiding causing corundum crucible to break, heating process is adjusted heating rate and control smelting temperature according to different crucible size and compound amount by changing the induction furnace output rating.Heat-processed is divided 5 sections at least, first section mixture temperature rises to 500～600 ℃ by room temperature, second section mixture temperature rises to 800～850 ℃, the 3rd section mixture temperature rises to 1000～1050 ℃, the 4th section mixture temperature rises to 1100～1150 ℃, the 5th section mixture temperature rises to the glass smelting temperature, and total heating process time can effectively be controlled at 60～90 minutes.
In sum, the present invention utilizes the graphite jacket as heating element, and it is non-conductive to have solved frit, athermic defective in induction furnace; Adopt the mode of induction heating, heat-up rate is fast, reduces the volatilization of glass ingredient in the process of founding, and reduces the pollution to environment, and the glass powder that assurance is made and the composition of design differ less, effectively guarantee the stability of glass powder composition; Production cost is low, the production efficiency height, and the composition of finished product conforms to design substantially.Be suitable for suitability for industrialized production.
Description of drawings
Accompanying drawing 1 is the SEM electromicroscopic photograph of the glass powder prepared of the embodiment of the invention 1.
As can be seen from Figure 1 the size distribution of glass powder is at 2.5～5 microns.
Embodiment
Do further explanation below in conjunction with accompanying drawing and specific examples:
Embodiment 1 preparation Pb-Si-Al-Zn-Ti-O system glass powder
Glass powder prepares according to the following steps:
1, the weight percent according to following component prescription takes by weighing each raw material: PbO 75%, SiO
215%, Al
2O
36%, ZnO 3%, TiO 1%.And fully mix, obtain 1 kilogram of compound;
2, compound is put into the 1 liter of corundum crucible that has the graphite jacket, utilizing effective furnace volume is that 5 liters induction furnace heats it.
Heating process: the induction furnace output rating is adjusted to 20KW, makes the glass compound by 50 ℃/minute heating rate, is heated to 550～600 ℃ within 10～12 minutes; Output rating is adjusted to 30KW, makes the glass compound by 30 ℃/minute heating rate, is heated to 800～830 ℃ within 10～12 minutes; Output rating is adjusted to 40KW, makes the glass compound by 20 ℃/minute heating rate, is heated to 1000～1020 ℃ within 10～12 minutes; Output rating is adjusted to 45KW, makes the glass compound by 15 ℃/minute heating rate, is heated to 1100～1120 ℃ within 6～8 minutes; Output rating is adjusted to 50KW, makes the glass compound by 12 ℃/minute heating rate, is heated to 1200 ℃ within 10～12 minutes; Treat that the glass compound melts fully, form fining glass liquid, turn off induction furnace, prepare shrend;
3, the glass metal after will melting is poured shrend in the deionized water into;
4, granular glass, abrading-ball and alcohol are put into ball mill according to 0.5: 0.8: 1 ratio and carry out ball milling, ball-milling technology is: 25 hours ball milling time, rotating speed is 280 rev/mins;
5, the oven dry of the glass powder behind the ball milling, classification being obtained D50 is 2.5 microns, and D90 is 4 microns palladium powder and packs.
Embodiment 2 preparation Pb-Si-Al-Zn-Ti-O system glass powder
Glass powder prepares according to the following steps:
1, the weight percent according to following component prescription takes by weighing each raw material: PbO 75%, SiO
215%, Al
2O
36%, ZnO 3%, TiO 1%.And fully mix, obtain 2 kilograms of compounds;
2, compound is put into 2 liters of corundum crucibles that have the graphite jacket, utilizing effective furnace volume is that 5 liters induction furnace heats it.
Heating process: the induction furnace output rating is adjusted to 25KW, makes the glass compound by 48 ℃/minute heating rate, is heated to 550～600 ℃ within 10～12 minutes; Output rating is adjusted to 30KW, makes the glass compound by 32 ℃/minute heating rate, is heated to 800～830 ℃ within 8～10 minutes; Output rating is adjusted to 38KW, makes the glass compound by 22 ℃/minute heating rate, is heated to 1000～1020 ℃ within 10～12 minutes; Output rating is adjusted to 45KW, makes the glass compound by 15 ℃/minute heating rate, is heated to 1100～1120 ℃ within 8～10 minutes; Output rating is adjusted to 50KW, makes the glass compound by 13 ℃/minute heating rate, is heated to 1250 ℃ within 8～10 minutes; Treat that the glass compound melts fully, form fining glass liquid, turn off induction furnace, prepare shrend;
3, the glass metal after will melting is poured shrend in the deionized water into;
4, granular glass, abrading-ball and alcohol are put into ball mill according to 1: 1: 1.5 ratio and carry out ball milling, ball-milling technology is: 20 hours ball milling time, rotating speed is 320 rev/mins;
5, the oven dry of the glass powder behind the ball milling, classification being obtained D50 is 2.6 microns, and D90 is 4.2 microns palladium powder and packs.
1, the weight percent according to following component prescription takes by weighing each raw material: Bi
2O
330%, SiO
230%, Al
2O
315%, ZnO 10%, B
2O
310%, MgO 5%.And fully mix, obtain 1 kilogram of compound;
2, compound is put into the 1 liter of corundum crucible that has the graphite jacket, utilizing effective furnace volume is that 5 liters induction furnace heats it.
Heating process: the induction furnace output rating is adjusted to 25KW, makes the glass compound by 50 ℃/minute heating rate, is heated to 550～600 ℃ within 10～12 minutes; Output rating is adjusted to 30KW, makes the glass compound by 40 ℃/minute heating rate, is heated to 800～830 ℃ within 8～10 minutes; Output rating is adjusted to 38KW, makes the glass compound by 30 ℃/minute heating rate, is heated to 1030～1050 ℃ within 12～15 minutes; Output rating is adjusted to 45KW, makes the glass compound by 20 ℃/minute heating rate, is heated to 1130～1150 ℃ within 10～12 minutes; Output rating is adjusted to 50KW, makes the glass compound by 14 ℃/minute heating rate, is heated to 1500 ℃ within 24～30 minutes; Treat that the glass compound melts fully, form fining glass liquid, turn off induction furnace, prepare shrend;
3, the glass metal after will melting is poured shrend in the deionized water into;
4, granular glass, abrading-ball and alcohol are put into ball mill according to 1: 1: 1.5 ratio and carry out ball milling, ball-milling technology is: 20 hours ball milling time, rotating speed is 320 rev/mins;
5, the oven dry of the glass powder behind the ball milling, classification being obtained D50 is 2.8 microns, and D90 is 4.2 microns palladium powder and packs.
Embodiment 4 preparation Bi-Si-B-Zn-Al-Mg-O system glass
1, the weight percent according to following component prescription takes by weighing each raw material: Bi
2O
330%, SiO
230%, Al
2O
315%, ZnO 10%, B
2O
310%, MgO 5%.And fully mix, obtain 2 kilograms of compounds;
2, compound is put into 2 liters of corundum crucibles that have the graphite jacket, utilizing effective furnace volume is that 5 liters induction furnace heats it.
Heating process: the induction furnace output rating is adjusted to 25KW, makes the glass compound by 40 ℃/minute heating rate, is heated to 550～600 ℃ within 12～18 minutes; Output rating is adjusted to 30KW, makes the glass compound by 32 ℃/minute heating rate, is heated to 800～830 ℃ within 10～12 minutes; Output rating is adjusted to 40KW, makes the glass compound by 22 ℃/minute heating rate, is heated to 1030～1050 ℃ within 12～15 minutes; Output rating is adjusted to 48KW, makes the glass compound by 15 ℃/minute heating rate, is heated to 1130～1150 ℃ within 8～10 minutes; Output rating is adjusted to 55KW, makes the glass compound by 13 ℃/minute heating rate, is heated to 1600 ℃ within 45～50 minutes; Treat that the glass compound melts fully, form fining glass liquid, turn off induction furnace, prepare shrend;
3, the glass metal after will melting is poured shrend in the deionized water into;
4, granular glass, abrading-ball and alcohol are put into ball mill according to 1.2: 1.5: 2 ratio and carry out ball milling, ball-milling technology is: 10 hours ball milling time, rotating speed is 350 rev/mins;
5, the oven dry of the glass powder behind the ball milling, classification being obtained D50 is 2.7 microns, and D90 is 4.2 microns palladium powder and packs.
Comparative example in the table 1 is to adopt conventional process to prepare glass powder.By analyzing production cost, production cycle and the recovery rate between comparative example and the embodiment, as can be known from Table 1, utilize the described novel process of patent of the present invention to prepare glass powder and have clear superiority.
Table 1
Claims (2)
1. the preparation technology of a solar cell size usefulness palladium powder comprises the steps:
The first step: batching
Component prescription by design takes by weighing each raw material, mixes, and obtains compound;
Second step: heat fused
The first step gained compound is put into the corundum crucible that has the graphite jacket, at the induction furnace internal heating to temperature of fusion 1200-1700 ℃; Heat fused divides five stages to finish,
First section, mixture temperature rises to 500～600 ℃ by room temperature, and temperature rise rate is 40-50 ℃/minute;
Second section, mixture temperature rises to 800～850 ℃, and temperature rise rate is 30-40 ℃/minute;
The 3rd section, mixture temperature rises to 1000～1050 ℃, and temperature rise rate is 20-30 ℃/minute;
The 4th section, mixture temperature rises to 1100～1150 ℃, and temperature rise rate is 15-20 ℃/minute;
The 5th section, mixture temperature rises to the glass melting temperature, and temperature rise rate is 10-15 ℃/minute;
The 3rd step: broken after the shrend
Pour the glass metal that second step obtained in deionized water shrend; Ball milling is 2.5～3.0 microns to D50 then, and D90 is 4～5 microns; Dry, sieve and pack.
2. a kind of solar cell size according to claim 1 is with the preparation technology of palladium powder, it is characterized in that: described ball milling adopts wet ball-milling, ball-milling medium is alcohol, material, abrading-ball and alcohol are put into ball mill according to the ratio of 0.5～1.2:0.8～1.5:1～2 and are carried out ball milling, ball-milling technology is: 10～25 hours ball milling time, rotating speed is 280～350 rev/mins.
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| CN103233264A (en) * | 2013-05-03 | 2013-08-07 | 江苏海翔化工有限公司 | Silicon material melting heating process capable of preventing silicon leakage in quartz crucible in Czochralski method |
| CN104658634B (en) * | 2015-02-03 | 2017-01-18 | 四川银河星源科技有限公司 | Crystalline silicon solar battery back electrode silver paste and preparation method thereof |
| CN112791801A (en) * | 2020-12-18 | 2021-05-14 | 中国振华集团云科电子有限公司 | Method for improving quality consistency of glass powder |
Citations (4)
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|---|---|---|---|---|
| CN1903763A (en) * | 2006-08-09 | 2007-01-31 | 中国建筑材料科学研究总院 | Glass scintillator for thermal neutron detection and its preparation method |
| CN101195516A (en) * | 2006-12-06 | 2008-06-11 | 长沙理工大学 | Low-melting point leadless crystallizing glass for sealing high temperature electric heating tube and technique of preparing the same |
| CN101549957A (en) * | 2009-03-23 | 2009-10-07 | 东华大学 | Bi*O*-B*O* series lead-free glass powder for electronic slurry and preparation method thereof |
| CN101560060A (en) * | 2009-05-08 | 2009-10-21 | 苏州晶讯科技股份有限公司 | Surface treatment method of low temperature glass for solar cell conductive slurry |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1903763A (en) * | 2006-08-09 | 2007-01-31 | 中国建筑材料科学研究总院 | Glass scintillator for thermal neutron detection and its preparation method |
| CN101195516A (en) * | 2006-12-06 | 2008-06-11 | 长沙理工大学 | Low-melting point leadless crystallizing glass for sealing high temperature electric heating tube and technique of preparing the same |
| CN101549957A (en) * | 2009-03-23 | 2009-10-07 | 东华大学 | Bi*O*-B*O* series lead-free glass powder for electronic slurry and preparation method thereof |
| CN101560060A (en) * | 2009-05-08 | 2009-10-21 | 苏州晶讯科技股份有限公司 | Surface treatment method of low temperature glass for solar cell conductive slurry |
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