CN103601369B - Preparation method of the solaode back aluminum slurry with lead-free electronic glass powder - Google Patents
Preparation method of the solaode back aluminum slurry with lead-free electronic glass powder Download PDFInfo
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- CN103601369B CN103601369B CN201310555306.9A CN201310555306A CN103601369B CN 103601369 B CN103601369 B CN 103601369B CN 201310555306 A CN201310555306 A CN 201310555306A CN 103601369 B CN103601369 B CN 103601369B
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Abstract
The present invention relates to a kind of preparation method of solaode back aluminum slurry with lead-free electronic glass powder.Aluminium paste used for solar batteries, Main System have：Bi2O3‑B2O3‑SiO2、V2O5‑B2O3‑ZnO、BaO‑B2O3ZnO etc., such material system coefficient of expansion are larger, want to reduce the coefficient of expansion, and material melting point will be raised.The present invention solaode back aluminum slurry lead-free electronic glass powder preparing raw material and its weight proportion be：Bi2O330～90 parts；10～60 parts of ZnO；B2O310～30 parts；CaCO33 ~ 5 parts;WO32 ~ 8 parts；Al2O31 ~ 5 part;In2O30 ~ 1 part；ZrO20～2 part；BaCO30 ~ 5 part；P2O50～2 part；0～5 part of MgO；SiO20 ~ 10 part.Lead-free electronic glass powder excellent electrical properties prepared by the present invention, fusing point is low, thermal coefficient of expansion is little, electricity conversion is high, and, little angularity strong with crystal silicon adhesive force, water boiling resistance, leakage current are little；And harm will not be produced aborning to human body, harmful exhaust and waste water and waste residue is not produced.
Description
Technical field
The invention belongs to technical field of electronic materials, is related to a kind of solaode back aluminum slurry lead-free electronic glass powder
Preparation method.
Background technology
Aluminium paste used for solar batteries is that the high-performance developed for silk screen printing silicon solar cell back face electrode is led
Electrit is starched.Aluminium paste has good printing, electric conductivity, weatherability and chemical-resistance.Can with front electrode slurry co-sintering,
After sintering, silicon chip adhesive force is good, and silicon chip deformation is little, and aluminium film compactness is good, non-microcracked, not beading, can obtain splendid photoelectricity
Transformation efficiency, is preferable backplate slurry.The core technology of aluminium paste is the development of glass dust.In known technology,
Electronic devices and components, electron tube, semiconductor device encapsulating, the electronic glass of sealing-in are widely used in, are all to adopt PbO- at present
B2O3-SiO2、PbO-ZnO-B2O3Material system, the material system sealing property are good, and electrical property is good, moderate, are mesh
The main flow of front seal glass.The subject matter of presence is that lead content is high, consumption 50%～80%, in the production process of glass,
Greatly harm is caused to the healthy and environment of operator；The discarded element of sealing-in, PbO again can it is molten to rainwater,
In soil, bigger harm is caused to environment.In order to reduce the harm to human body, environment, develop without leaded joint again both at home and abroad
Glass material system, Main System have：Bi2O3-B2O3-SiO2、V2O5-B2O3-ZnO、BaO-B2O3- ZnO etc., three kinds of material bodies
It is excessive to there is the coefficient of expansion in system, wants to reduce the coefficient of expansion, and material melting point will be raised.
The content of the invention
It is an object of the invention to provide a kind of excellent electrical properties, fusing point is low, thermal coefficient of expansion is relatively low, and silicon chip adhesion
By force, preparation of the solaode back aluminum slurry that electricity conversion is higher, water boiling resistance, leakage current are little with lead-free electronic glass powder
Method.
The technical solution adopted in the present invention is：
Preparation method of the solaode back aluminum slurry with lead-free electronic glass powder, the solaode back aluminum slurry are used
The weight proportion of the preparing raw material of lead-free electronic glass powder is：
Bi2O330～90 parts；10～60 parts of ZnO；
B2O310～30 parts； CaCO33 ~ 5 parts;
WO32 ~ 8 parts； Al2O31 ~ 5 part;
Using the preparation method of above-mentioned material
（1）By various material precises, batch mixing 30 ~ 60 minutes in batch mixer；
（2）Glass-melting furnace is installed into crucible, 1000 ~ 1400 DEG C of predetermined temperature is warmed up to, is fed；
（3）After glass melting is uniform, scooped out with rustless steel spoon, slowly poured in water quenching pool；
（4）Water is put only, material is taken out, is loaded in jar mill, ball milling 60 ~ 72 hours, 300 mesh sieves are crossed in discharging；
（5）Slurry is put in the stainless steel cask of dispersion machine, addition is not less than the deionized water of 2 times of volumes of slurry, uses and divide
Scattered machine is stirred 30 ~ 60 minutes, static 12 hours, scoops upper strata clear water；So repeat 3 ~ 5 times；
（6）Dried 8～15 hours with 120 DEG C～150 DEG C in drying baker；
（7）It is broken, weigh, packaging.
Preparation method of the described solaode back aluminum slurry with lead-free electronic glass powder, solaode back aluminum slurry
Weight proportion with lead-free electronic glass powder is：
BaCO30 ~ 5 part； P2O50～2 part；
0～5 part of MgO； SiO2 0 ~ 10 part；
ZrO20～2 part.
Preparation method of the described solaode back aluminum slurry with lead-free electronic glass powder, solaode back aluminum slurry
Weight proportion with lead-free electronic glass powder is：
Bi2O350 parts；20 parts of ZnO；
B2O310 parts； CaCO35 parts;
WO32 parts； Al2O31.5 part;
BaCO31 part； P2O52 parts；
3 parts of MgO； SiO2 3 parts；
ZrO22 parts.
Preparation method of the described solaode back aluminum slurry with lead-free electronic glass powder, step（7）Add after middle weighing
Enter 0～1 part of In2O3After pack.
, relative to prior art, its advantage is as follows for the present invention：
Using lead-free environment-friendly materials, harm will not be produced aborning to human body, harmful exhaust and waste water is not produced
And waste residue, it is a kind of raw material environmental protection, production process environmental protection, the environmentally friendly new material of product environmental protection；Glass dust electrical resistance
Can be excellent, fusing point is little, thermal coefficient of expansion is little, adhesive force is high, leakage current is little, photoelectric transformation efficiency is high.
Specific embodiment
The present invention is aiming at that above-mentioned material system is leaded, thermal coefficient of expansion is too high, electricity conversion is low, not water boiling resistance
Put forward.The present invention is described in detail with reference to the accompanying drawings and detailed description.
（1）The constituent of material, the proportioning content of each composition
The present invention is made up of following material and its content：
Bi2O330～90 parts；10～60 parts of ZnO；
B2O310～30 parts； CaCO33 ~ 5 parts;
WO32 ~ 8 parts； Al2O31 ~ 5 part;
In2O3 0 ~ 1 part； ZrO20～2 part；
BaCO3 0 ~ 5 part； P2O50～2 part；
0～5 part of MgO； SiO2 0 ~ 10 part.
（2）Effect of each composition in prescription, the selection reason of content, the scientific theory that each composition is combined
The know-why of this project institute foundation is：
In the glass that we can contact, can form glass network generally has three kinds of materials：SiO2, B2O3, P2O5, they
It is used alone or as a mixture, becomes the base substance to form glass.And the structure of glass have at present two kinds it is theoretical：Network theory and
Matted crystal theory.In glass, in order to adjust the property of glass, other oxides are commonly incorporated into, these materials can be divided into two classes：One class
It is the body that scores a goal, such as K2O、Na2O, CaO, MgO, BaO etc., their addition destroy the network structure of glass, make the bonding of glass
Fracture, at high temperature viscosity reduction；Another kind of is androgyne, such as PbO, Al2O3, under certain conditions, it is the body that scores a goal, and another
In the case of outer, it is glass former.This project selects B2O3As basic glass forming substance matter, it is due to B2O3With low
Fusing point feature, B2O3Liquid can be melt at 450 DEG C, and SiO2Fusing point at 1680 DEG C；In order to reduce the expansion system of glass
Number, adds Zinc Oxide again.From Bi2O3It is because that bismuth metal and lead, in same period, are positioned proximate to, the property phase of oxide
Closely.As the chemical stability of bismuth glass is substantially not so good as lead glass, in order to improve the chemical stability of bismuthates, in material system
A part of bismuth oxide be instead of with alkali metal oxide, while adding a small amount of aluminium oxide and zirconium dioxide.In order to improve material
Electricity conversion, add a small amount of Tungstic anhydride., as tungsten ion is sexavalence, forms donor doping with tetravalence silicon, can increase
Plus photoelectron quantity, improve transformation efficiency.
The theory innovation of this project is the main material from the relatively low raw material bismuth oxide of fusing point as formula, not leaded
Deng harmful substance.More Zinc Oxide is added simultaneously, on the one hand reducing the high-temperature viscosity of material, on the other hand can also be reduced
The coefficient of expansion of material.This is because the coefficient of expansion and its fusing point of general glass --- using temperature in inverse ratio, want to obtain
Low-melting glass material, the coefficient of expansion of material will be big, and Zinc Oxide is a kind of unique fusing point that can both reduce material, and
The oxide of the coefficient of expansion of material can be reduced.The linear expansion coefficient of glass is available plus approximately calculates with formula：
α glass=α1P1+α2P2+α3P3+……
In formula：The linear expansion coefficient of α glass --- glass；
P1,P2... each oxide weight percentage composition in glass；
α1, α2... the linear expansion coefficient of each oxide（Test value）.
Silicon dioxide is added again in formula, due to boron oxide unstable chemcial property, silica chemistry is steady
It is fixed, therefore a small amount of silicon dioxide is added, improve the chemical stability of material system.In material prescription, in order to reduce glass
Fusing point, add a small amount of phosphorus pentoxide again, this is that, due to phosphorus pentoxide chemical property extremely unstable, therefore its consumption is not
It is preferably excessive.
The formula of principle design according to this, at 480 DEG C, the coefficient of expansion, can be with crystal silicon in 6.0ppm or so for the fusing point of glass
The coefficient of expansion of matrix reaches best fit.
（3）A kind of preparation method of the material is given below：
1st, precise is carried out by above-mentioned material, be accurate to 1g, batch mixing 30 ~ 60 minutes in batch mixer；
2nd, glass-melting furnace is installed into crucible, is warmed up to 1100 DEG C of predetermined temperature, fed；
3rd, after glass melting is uniform, scooped out with rustless steel spoon, slowly poured in water quenching pool；
4th, Jiang Shui is put only, takes out material, loads in jar mill, and jar mill is previously charged into the ballstone of constant weight；Ball-milling Time
For 60 ~ 72h, discharging, 300 mesh sieves are crossed；Slurry is put in the stainless steel cask of dispersion machine, addition is not less than 2 times of volumes of slurry
Deionized water, starts dispersion machine, stirs 30 ~ 60 minutes.Static 12h, scoops upper strata clear water.So repeat 3 ~ 5 times；
5th, 120 DEG C～150 DEG C 8～15h of drying in drying baker；
6th, crush, weigh, 0 ~ 1 part of In of outer addition2O3Mix homogeneously, packaging.
（4）Material property prepared by the preparation method according to the present invention is as follows：
Color：Light red；
Granularity：d50=1~2μm；
Softening temperature：Tg=440℃；
Sealing temperature：480 DEG C～550 DEG C；
Resistance to water：(0.010～0.027) mg/cm2；
Bulk density：(5.232～5.501) g/cm3；
Thermal coefficient of expansion：（5.80～6.25）×10-7℃-1。
The aluminium paste performance prepared with this glass dust is as follows（By taking 5 inches of silicon chip as an example）：
Electricity conversion：η=18.6%；
Angularity：≤1.0mm；
Adhesive force：The vertical pull-up of pressure sensitive adhesive tape, aluminium lamination are not peeled off from silicon chip；
Boiling test：85 ~ 100 DEG C of hot water, 30 ~ 60 minutes, aluminium lamination was non-foaming, did not fell off.
Embodiment 1：
1st, formula
Bi2O350 parts；20 parts of ZnO；
B2O310 parts； CaCO35 parts;
WO32 parts； Al2O31.5 part;
BaCO3 1 part； P2O52 parts；
3 parts of MgO； SiO2 3 parts；
ZrO22 parts. In2O3 0.5 part.
Precise is carried out by above-mentioned material proportioning, gross weight is 1Kg.
2nd, batch mixing is in V-type batch mixer batch mixing 20min；
3rd, crucible is put in melting in crucible furnace well, and programmed is warmed up to 1100 DEG C, charging, is connect after 20min for the second time
Material, being filled it up with crucible, then is taken out after melting 20min, is poured slowly in the container equipped with water.
4th, Jiang Shui is put only, takes out material, loads in jar mill, and jar mill is previously charged into the ballstone of constant weight；Ball-milling Time
For 60 ~ 72h, discharging, 300 mesh sieves are crossed；Slurry is put in the stainless steel cask of dispersion machine, addition is not less than 2 times of volumes of slurry
Deionized water, starts dispersion machine, stirs 30 ~ 60 minutes.Static 12h, scoops upper strata clear water.So repeat 3 ~ 5 times；
5th, 120 DEG C～150 DEG C 8～15h of drying in drying baker；
6th, crush, weigh, 0 ~ 1 part of In of outer addition2O3Mix homogeneously, packaging.
Embodiment 2：
1st, formula
Bi2O360 parts；10 parts of ZnO；
B2O310 parts； CaCO33 parts;
WO32 parts； Al2O31.5 part;
BaCO3 3 parts； P2O52 parts；
3 parts of MgO； SiO2 3 parts；
ZrO22 parts. In2O3 0.5 part.
Precise is carried out by above-mentioned material proportioning, gross weight is 1Kg.
2nd, batch mixing is in V-type batch mixer batch mixing 20min；
3rd, crucible is put in melting in crucible furnace well, and programmed is warmed up to 1100 DEG C, charging, is connect after 20min for the second time
Material, being filled it up with crucible, then is taken out after melting 20min, is poured slowly in the container equipped with water.
4th, Jiang Shui is put only, takes out material, loads in jar mill, and jar mill is previously charged into the ballstone of constant weight；Ball-milling Time
For 60 ~ 72h, discharging, 300 mesh sieves are crossed；Slurry is put in the stainless steel cask of dispersion machine, addition is not less than 2 times of volumes of slurry
Deionized water, starts dispersion machine, stirs 30 ~ 60 minutes.Static 12h, scoops upper strata clear water.So repeat 3 ~ 5 times；
5th, 120 DEG C～150 DEG C 8～15h of drying in drying baker；
6th, crush, weigh, 0 ~ 1 part of In of outer addition2O3Mix homogeneously, packaging.
Embodiment 3：
1st, formula
Bi2O370 parts；10 parts of ZnO；
B2O310 parts； CaCO33 parts;
WO32 parts； Al2O31.5 part;
SiO2 2 parts； ZrO21 part；
In2O3 0.5 part.
Precise is carried out by above-mentioned material proportioning, gross weight is 1Kg.
2nd, batch mixing is in V-type batch mixer batch mixing 20min；
3rd, crucible is put in melting in crucible furnace well, and programmed is warmed up to 1100 DEG C, charging, is connect after 20min for the second time
Material, being filled it up with crucible, then is taken out after melting 20min, is poured slowly in the container equipped with water.
4th, Jiang Shui is put only, takes out material, loads in jar mill, and jar mill is previously charged into the ballstone of constant weight；Ball-milling Time
For 60 ~ 72h, discharging, 300 mesh sieves are crossed；Slurry is put in the stainless steel cask of dispersion machine, addition is not less than 2 times of volumes of slurry
Deionized water, starts dispersion machine, stirs 30 ~ 60 minutes.Static 12h, scoops upper strata clear water.So repeat 3 ~ 5 times；
5th, 120 DEG C～150 DEG C 8～15h of drying in drying baker；
6th, crush, weigh, 0 ~ 1 part of In of outer addition2O3Mix homogeneously, packaging.
Claims (1)
1. preparation method of the solaode back aluminum slurry with lead-free electronic glass powder, it is characterised in that：The solaode
The weight proportion of back aluminum slurry lead-free electronic glass powder is：
Bi2O330～90 parts；10～60 parts of ZnO；
B2O310～30 parts； CaCO33 ~ 5 parts;
WO32 ~ 8 parts； Al2O31 ~ 5 part;
In2O30 ~ 1 part； ZrO20～2 part；
BaCO30 ~ 5 part； P2O50～2 part；
0～5 part of MgO； SiO20 ~ 10 part；
Using the preparation method of above-mentioned material
（1）By various material precises, batch mixing 30～60 minutes in batch mixer；
（2）Glass-melting furnace is installed into crucible, 1000～1400 DEG C of predetermined temperature is warmed up to, is fed；
（3）After glass melting is uniform, scooped out with rustless steel spoon, slowly poured in water quenching pool；
（4）Water is put only, material is taken out, is loaded in jar mill, ball milling 60～72 hours, 300 mesh sieves are crossed in discharging；
（5）Glass dust is put in the stainless steel cask of dispersion machine, addition is not less than the deionized water of 2 times of volumes of glass dust, uses and divide
Scattered machine is stirred 30～60 minutes, static 12 hours, scoops upper strata clear water；So repeat 3～5 times；
（6）Dried 8～15 hours with 120 DEG C～150 DEG C in drying baker；
（7）It is broken, weigh, packaging.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105347688A (en) * | 2015-12-14 | 2016-02-24 | 周妙思 | Preparation method of glass powder for electronic paste |
| CN105502952A (en) * | 2015-12-14 | 2016-04-20 | 周妙思 | Glass powder |
| CN105417954A (en) * | 2015-12-14 | 2016-03-23 | 周妙思 | Unleaded glass powder |
| CN106219987B (en) * | 2016-07-25 | 2020-07-14 | 常州聚和新材料股份有限公司 | Glass material for silicon solar cell slurry, preparation method thereof and slurry |
| CN108238723A (en) * | 2016-12-26 | 2018-07-03 | 西安宏星电子浆料科技有限责任公司 | Solar energy crystal silicon battery back silver paste lead-free electronic glass powder and preparation method thereof |
| CN110423012B (en) * | 2019-08-09 | 2021-12-24 | 江苏国瓷泓源光电科技有限公司 | Glass powder for PERC aluminum paste and preparation method thereof |
| CN112960908B (en) * | 2021-02-04 | 2023-03-28 | 江苏日御光伏新材料科技有限公司 | Glass powder and preparation method thereof |
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| CN101913763A (en) * | 2010-08-21 | 2010-12-15 | 常州盈德能源科技有限公司 | Glass composite for back surface field aluminum paste of solar battery and preparation method thereof |
| CN102757182A (en) * | 2012-08-06 | 2012-10-31 | 西安创联宏晟电子有限公司 | Low-temperature low expansion coefficient high-rigidity lead-free electronic glass powder and preparation method thereof |
| CN102898026A (en) * | 2012-08-22 | 2013-01-30 | 广州市儒兴科技开发有限公司 | Lead-free inorganic adhesive used in silver paste on crystalline silicon solar cell back, and preparation method thereof |
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| JP2743332B2 (en) * | 1989-08-17 | 1998-04-22 | 日本電気硝子株式会社 | Sealing material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101913763A (en) * | 2010-08-21 | 2010-12-15 | 常州盈德能源科技有限公司 | Glass composite for back surface field aluminum paste of solar battery and preparation method thereof |
| CN102757182A (en) * | 2012-08-06 | 2012-10-31 | 西安创联宏晟电子有限公司 | Low-temperature low expansion coefficient high-rigidity lead-free electronic glass powder and preparation method thereof |
| CN102898026A (en) * | 2012-08-22 | 2013-01-30 | 广州市儒兴科技开发有限公司 | Lead-free inorganic adhesive used in silver paste on crystalline silicon solar cell back, and preparation method thereof |
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Address after: 710065 No. 3 904 Factory Building of Zhangbajie Electronic West Street, Xi'an High-tech Zone, Shaanxi Province Patentee after: Xi'an Hongxing Electronic Slurry Technology Co.,Ltd. Address before: 710075 block D, building No. 16, high tech Road, high tech Zone, Shaanxi, Xi'an, No. five Patentee before: Xi'an Hongxing Electronic Slurry Technology Co.,Ltd. |