CN106746686A - A kind of high temperature resistant aluminium paste glass dust and preparation method thereof - Google Patents
A kind of high temperature resistant aluminium paste glass dust and preparation method thereof Download PDFInfo
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- CN106746686A CN106746686A CN201710034691.0A CN201710034691A CN106746686A CN 106746686 A CN106746686 A CN 106746686A CN 201710034691 A CN201710034691 A CN 201710034691A CN 106746686 A CN106746686 A CN 106746686A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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Abstract
The invention discloses a kind of high temperature resistant aluminium paste glass dust, including following weight/mass percentage composition raw material:Bi2O310~50%, B2O35~50%, SiO20.1~5%, Al2O30.1~2%, ZnO 5~20%, alkaline earth oxide 1~20%, V2O5、P2O5、Sb2O3、MoO3、WO3And Cr2O3In the combination 0.1~15% of one or more.There is high temperature aluminum bud, the electrically technical problem such as reduction, water boiling resistance performance deficiency without chemical stability is good, softening point is high, the short, wetability of material property is good after solving existing aluminium paste high temperature sintering in the glass dust.The invention also discloses the preparation method of above-mentioned high temperature resistant aluminium paste glass dust.
Description
Technical field
The invention belongs to back aluminum slurry technical field, and in particular to a kind of high temperature resistant aluminium paste glass dust and its preparation side
Method.
Background technology
, as back surface field to silicon chip back lifting passivation, different photovoltaic producers are due to using for crystal silicon solar energy battery aluminium paste
Positive silver-colored difference and cell piece difference in itself, can there are some differences in slurry sintering temperature, and the presence of these differences
Temperature-resistance characteristic to back field aluminum paste proposes requirement higher.
The composition of aluminium paste mainly has aluminium powder, inorganic bond, organic bond and different additives, and glass dust belongs to nothing
Machine adhesive.In known field, the composition of glass dust includes Network former, and Network modifier is (in the middle of network outer body and network
Body).B2O3As a kind of typical glass network former, [BO can be formed3] and [BO4]。SiO2It is also a kind of typical glass
Network is formed, and can form [SiO4]。Bi2O3Within the specific limits also can be as Network former, with [BiO4] form enter glass
In glass Network former, but this scope is narrow.Alkali metal oxide, as Network modifier, can play fluxing action, drop
The viscosity of eutectic melt body.Additionally, V2O3、Sb2O3、MoO3、Cr2O3Effectively can significantly reduce the surface of glass in glass Deng adding
Tension force.
The patent of Application No. 201310117504.7 is related to aluminium paste of the low warpage of a kind of high temperature resistant and preparation method thereof, annotates
A kind of raw material by low thermal coefficient of expansion has been released to add the expansion coefficient difference between balance aluminium lamination and matrix and reduce warpage
Method, its slurry sintering temperature characteristic do not describe specifically.The patent of Application No. 201210446525.9 discloses one
Aluminium paste lead-free glass powder is planted, by reducing Bi contents, improves wettability of the melten glass powder to silicon substrate.In glass material
Silicone content is up to more than 20%, SiO2The relative infusibility in frit system, the system smelting temperature is higher.
201410639588.5 patents disclose a kind of glass dust improves glass dust to aluminium by the introducing of sodium sulphate or niter cake
The characteristics of wettability of grain and silicon base, its glass dust is Al2O3Content is high, and sodium element easily forms compound in the semiconductors.
The patent of Application No. 201510249469.3 discloses the glass that a kind of bismuth high contains, although smelting temperature and softening point is low, but
The larger problem that bismuth glass high is present is that easy crystallization causes levelling bad.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of high temperature resistant aluminium paste glass dust, the glass dust chemically stable
Property good, softening point is high, the short, wetability of material property is good, can solve to occur after existing aluminium paste high temperature sintering high temperature aluminum bud, electrical reduction,
The problems such as water boiling resistance performance is not enough.
The present invention provides glass dust SiO in formula design2And Al2O3Content is low, and alkali gold is replaced with alkaline earth metal compound
The category fluxing reduction system smelting temperature of compound, while the impurity for reducing semiconductor is introduced.Glass formation range is wide, is difficult analysis
Crystalline substance, flow leveling is good after high-temperature fusion, can good wet, the fine and close journey after promoting aluminium lamination to sinter to silicon base and alumina particles
Degree.
The technical problems to be solved by the invention also reside in the preparation method for being to provide above-mentioned high temperature resistant aluminium paste glass dust,
The preparation method concise in technology, low cost.
First technical problem to be solved by this invention is achieved by the following technical solution:A kind of high temperature resistant aluminium
Slurry glass dust, including following weight/mass percentage composition raw material:Bi2O310~50%, B2O35~50%, SiO20.1~
5%, Al2O30.1~2%, ZnO 5~20%, alkaline earth oxide 1~20%, V2O5、P2O5、Sb2O3、MoO3、WO3With
Cr2O3In the combination 0.1~15% of one or more.
Preferably, the weight/mass percentage composition of each raw material is Bi2O310~50%, B2O310~40%, SiO20.1~
5%, Al2O30.1~2%, ZnO 5~20%, alkaline earth oxide 1~20%, V2O5、P2O5、Sb2O3、MoO3、WO3With
Cr2O3In the combination 5~15% of one or more.
Further, the weight/mass percentage composition of each raw material is Bi2O310~35%, B2O320~40%, SiO21~
5%, Al2O31~2%, ZnO 5~20%, alkaline earth oxide 1~20%, V2O5、P2O5、Sb2O3、MoO3、WO3With
Cr2O3In the combination 10~15% of one or more.
The present invention is designed and adjusted for glass dust above feature to formula, and Bi-B-Zn systems glass has outstanding
Acid-proof alkaline, can guarantee that aluminium paste sintering after water boiling resistance performance.Add appropriate SiO2、Al2O3Can further, lifting glass
Acidproof alkaline stability, and the infusibility of system will not be increased.The alkaline earth oxide reduction glass such as selection MgO, CaO
The material of glass can be reduced while viscosity, glass melting viscosity is just drastically reduced at a relatively high temperature.V2O5、P2O5
Component can increase the stability of glass structure, Sb2O3、MoO3、WO3、Cr2O3Component can reduce the surface tension lifting glass of glass
To alumina particles and the wettability of substrate.
The alkaline earth oxide includes that MgO and/or CaO, wherein MgO come from MgCO3, CaO is from CaCO3。
The Al2O3From Al (OH)3。
From hydroxide and carbonate, the active oxide high of generation can be first decomposed at high temperature, be conducive to
The carrying out of material reaction.
The softening point of glass dust of the present invention is 650~700 DEG C, granularity D50It is 1.5~4.0 μm.
Second technical problem to be solved by this invention is achieved by the following technical solution:Above-mentioned high temperature resistant aluminium
The preparation method of slurry glass dust, comprises the following steps:Each raw material is chosen, being placed in after mixing carries out melting, liquation in Muffle furnace
Dried after deionization water quenching and crushed, then carry out ball milling, dried, obtain final product high temperature resistant aluminium paste glass dust.
Temperature during melting is preferably 1000~1300 DEG C, and smelting time is preferably 30~120min.
Ball-milling medium is preferably deionized water during ball milling, and Ball-milling Time is preferably 10~20h, after slurry is stood after ball milling
Upper water is separated off, lower floor's material is dried in 115~125 DEG C of baking ovens, obtain final product high temperature resistant aluminium paste glass dust.
Compared with prior art, the present invention has advantages below:
(1) glass dust that the present invention is provided is characterized in that chemical stability is good, softening point is high, material as low-melting-point glass powder
The short, wetability of property is good;
(2) present invention provides glass dust SiO in formula design2And Al2O3Content is low, is replaced with alkaline earth metal compound
Alkali metal compound is introduced to reduce system smelting temperature and can reduce semiconductor impurities element, and glass formation range is wide, no
Easy crystallization, flow leveling is good after high-temperature fusion, can good wet, the densification after promoting aluminium lamination to sinter to silicon base and alumina particles
Degree;
(3) glass dust that the present invention is provided is applied has following advantage in aluminium paste:The good glass dust of chemical stability
The high-temperature resistant water that aluminium paste can be lifted boils performance;High softening-point glass dust just corrosion oxidation aluminium film at higher temperatures, material property is short
Glass dust to be in low viscosity flow dynamic time short, which reduce action time of the glass dust to alumina particles, control the excess of aluminium
Melt out and excessive alusil alloy reaction so that aluminium paste can bear sintering temperature higher and produce high temperature aluminum bud;Glass dust
Even if surface tension is low, moist can guarantee that glass dust in the short period of time also can be to alumina particles and silicon base effective wetting by force
Infiltration, lifts the compactness extent after the sintering of slurry.
Specific embodiment
The present invention is given specific description in each of the embodiments described below.These embodiments be all it is illustrative, not
The present invention is limited in any way.It will be understood by those skilled in the art that without departing from the spirit and scope of the invention
The details of technical solution of the present invention and form can be modified or replaced, but these modification and replacement each fall within it is of the invention
In protection domain.
Embodiment 1
The high temperature resistant aluminium paste glass dust that the present embodiment is provided, is made up of the raw material of following weight/mass percentage composition:
Bi2O335%th, B2O325%th, SiO23%th, Al2O30.1%th, ZnO 19.9%, MgO 5%, V2O52%th,
Sb2O310%.
Wherein MgO comes from MgCO3, Al2O3From Al (OH)3。
The preparation method of the high temperature resistant aluminium paste glass dust is as follows:
(1) by above-mentioned weight/mass percentage composition, by various raw material weighings after well mixed in batch mixer, mixed material
Crucible for smelting is put into, regulation smelting temperature is 1000~1300 DEG C, 30~120min of insulation melting;
(2) by the glass dregs after deionization water quenching, dried using 10~20h of deionized water ball milling, the glass paste after ball milling
Material is separated off upper water after standing, and is then dried in 115~125 DEG C of baking ovens, that is, high temperature resistant aluminium paste glass dust is obtained.
Embodiment 2
The high temperature resistant aluminium paste glass dust that the present embodiment is provided, is made up of the raw material of following weight/mass percentage composition:
Bi2O310%th, B2O350%th, SiO2 0.1、Al2O32%th, ZnO 15%, CaO 10%, V2O51.9%th,
Sb2O310%th, MoO31%.
Wherein CaO comes from CaCO3, Al2O3From Al (OH)3。
The preparation method of the high temperature resistant aluminium paste glass dust is with embodiment 1.
Embodiment 3
The high temperature resistant aluminium paste glass dust that the present embodiment is provided, is made up of the raw material of following weight/mass percentage composition:
Bi2O340%th, B2O313%th, SiO25%th, Al2O32%th, ZnO 5%, MgO 20%, P2O510%th, WO3
5%.
The preparation method of the high temperature resistant aluminium paste glass dust is with embodiment 1.
Embodiment 4
The high temperature resistant aluminium paste glass dust that the present embodiment is provided, is made up of the raw material of following weight/mass percentage composition:
Bi2O325%th, B2O340%th, SiO22%th, Al2O31%th, ZnO 16%, CaO 10%, P2O54%th, Cr2O3
2%.
The preparation method of the high temperature resistant aluminium paste glass dust is with embodiment 1.
Embodiment 5
The high temperature resistant aluminium paste glass dust that the present embodiment is provided, is made up of the raw material of following weight/mass percentage composition:
Bi2O330%th, B2O325%th, SiO23%th, Al2O32%th, ZnO 10%, MgO 7%, MgO 8%, V2O5
5%th, P2O55%th, MoO33%th, WO32%.
The preparation method of the high temperature resistant aluminium paste glass dust is with embodiment 1.
Embodiment 6
The high temperature resistant aluminium paste glass dust that the present embodiment is provided, is made up of the raw material of following weight/mass percentage composition:
Bi2O325%th, B2O345%th, SiO21%th, Al2O31%th, ZnO 12%, MgO 3%, Sb2O310%th, MoO3
3%.
The preparation method of the high temperature resistant aluminium paste glass dust is with embodiment 1.
Embodiment 7
The high temperature resistant aluminium paste glass dust that the present embodiment is provided, is made up of the raw material of following weight/mass percentage composition:
Bi2O338%th, B2O320%th, SiO23%th, Al2O32%th, ZnO 8%, MgO 7%, CaO 7%, P2O5
2%th, Sb2O38%th, Cr2O35%.
The preparation method of the high temperature resistant aluminium paste glass dust is with embodiment 1.
Comparative example 1
The high temperature resistant aluminium paste glass dust that the present embodiment is provided, is made up of the raw material of following weight/mass percentage composition:
Bi2O350%th, B2O330%th, SiO24%th, Al2O31%th, ZnO 15%.
The specific implementation formula of embodiment 1-7 and comparative example 1 is as shown in table 1 below.
The specific consumption of the embodiment 1-7 of table 1 and comparative example 1
The detection of the glass dust of embodiment 8
Using American-European gram of laser particle size analyzer wet method test unorganic glass powder sample median particle diameter D50, using high temperature Muffle furnace
Test the softening point of glass dust.Test result is as shown in table 2.
The softening point detection of the embodiment 1-7 of table 2 and comparative example 1
As can be seen from Table 2, the glass dust in embodiment 1-7 and the glass dust in comparative example 1, softening point have increasing
Plus, but glass dust in embodiment 1-7 softens that melt temperature is high, causes the time of corrosion shorter to alumina particles and silicon base, slurry
Material has heat resistance higher.
Performance of the glass dust of embodiment 9 in aluminium paste
Cell piece is sintered using BTU sintering furnaces, 790~810 DEG C of true peak temperature, observation cell piece is apparent;At 75 DEG C
Deionized water in, soak cell piece, the response situation of aluminium back surface field is observed, as a result such as table 3 below.
Cell piece the apparent phenomenon in the embodiment 1-7 of table 3 and comparative example
A part of specific embodiment is enumerated above, and the present invention will be described, it is necessary to it is pointed out here that be the specifically real above
Apply example and be served only for that the invention will be further described, do not represent limiting the scope of the invention.Other people are according to the present invention
Some the nonessential modifications and adjustment made still fall within protection scope of the present invention.
Claims (9)
1. a kind of high temperature resistant aluminium paste glass dust, it is characterized in that the raw material including following weight/mass percentage composition:Bi2O310~
50%, B2O35~50%, SiO20.1~5%, Al2O30.1~2%, ZnO 5~20%, alkaline earth oxide 1~
20%, V2O5、P2O5、Sb2O3、MoO3、WO3And Cr2O3In the combination 0.1~15% of one or more.
2. high temperature resistant aluminium paste glass dust according to claim 1, it is characterized in that the weight/mass percentage composition of each raw material is
Bi2O310~50%, B2O310~40%, SiO20.1~5%, Al2O30.1~2%, ZnO 5~20%, alkaline-earth metal
Oxide 1~20%, V2O5、P2O5、Sb2O3、MoO3、WO3And Cr2O3In the combination 5~15% of one or more.
3. high temperature resistant aluminium paste glass dust according to claim 1, it is characterized in that the weight/mass percentage composition of each raw material is
Bi2O310~35%, B2O320~40%, SiO21~5%, Al2O31~2%, ZnO 5~20%, alkaline-earth metal oxide
Thing 1~20%, V2O5、P2O5、Sb2O3、MoO3、WO3And Cr2O3In the combination 10~15% of one or more.
4. the high temperature resistant aluminium paste glass dust according to claim any one of 1-3, it is characterized in that:The alkaline-earth metal oxide
Thing includes that MgO and/or CaO, wherein MgO come from MgCO3, CaO is from CaCO3。
5. the high temperature resistant aluminium paste glass dust according to claim any one of 1-3, it is characterized in that:The Al2O3From Al
(OH)3。
6. the high temperature resistant aluminium paste glass dust according to claim any one of 1-3, it is characterized in that:The softening of the glass dust
Point is 650~700 DEG C, granularity D50It is 1.5~4.0 μm.
7. the preparation method of the high temperature resistant aluminium paste glass dust described in any one of claim 1-3, it is characterized in that including following step
Suddenly:Each raw material is chosen, being placed in after mixing carries out melting in Muffle furnace, liquation is dried after deionization water quenching and crushed, and is then carried out
Ball milling, drying, obtains final product high temperature resistant aluminium paste glass dust.
8. the preparation method of high temperature resistant aluminium paste glass dust according to claim 6, it is characterized in that:Temperature during melting is
1000~1300 DEG C, smelting time is 30~120min.
9. the preparation method of high temperature resistant aluminium paste glass dust according to claim 6, it is characterized in that:Ball-milling medium during ball milling
It is deionized water, Ball-milling Time is 10~20h, upper water is separated off after slurry is stood after ball milling, by lower floor's material 115
Dried in~125 DEG C of baking ovens, obtain final product high temperature resistant aluminium paste glass dust.
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Cited By (6)
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CN107673623A (en) * | 2017-08-28 | 2018-02-09 | 广州市儒兴科技开发有限公司 | A kind of two-sided PERC aluminium pastes glass dust and preparation method thereof |
CN107673601A (en) * | 2017-08-28 | 2018-02-09 | 广州市儒兴科技开发有限公司 | A kind of PERC aluminium pastes glass dust and preparation method thereof |
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CN108529888A (en) * | 2018-04-02 | 2018-09-14 | 海宁市丁桥镇永畅知识产权服务部 | The preparation method of high temperature resistant aluminium paste glass powder |
CN115557706A (en) * | 2022-09-24 | 2023-01-03 | 江苏拜富科技股份有限公司 | Preparation process of high-performance glass powder |
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CN105632590A (en) * | 2016-03-18 | 2016-06-01 | 苏州开元民生科技股份有限公司 | Crystal silicon solar cell aluminum paste and preparation method therefor |
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CN102097154A (en) * | 2010-11-25 | 2011-06-15 | 长沙族兴金属颜料有限公司 | Back surface field aluminium paste for solar cells |
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CN107673623A (en) * | 2017-08-28 | 2018-02-09 | 广州市儒兴科技开发有限公司 | A kind of two-sided PERC aluminium pastes glass dust and preparation method thereof |
CN107673601A (en) * | 2017-08-28 | 2018-02-09 | 广州市儒兴科技开发有限公司 | A kind of PERC aluminium pastes glass dust and preparation method thereof |
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CN107673601B (en) * | 2017-08-28 | 2019-10-18 | 广州市儒兴科技开发有限公司 | A kind of PERC aluminium paste glass powder and preparation method thereof |
CN107746182B (en) * | 2017-08-28 | 2020-06-02 | 广州市儒兴科技开发有限公司 | Glass powder for high-electric-property crystalline silicon solar cell aluminum paste and preparation method thereof |
CN107673623B (en) * | 2017-08-28 | 2020-09-15 | 广州市儒兴科技开发有限公司 | Glass powder for double-sided PERC aluminum paste and preparation method thereof |
CN108529888A (en) * | 2018-04-02 | 2018-09-14 | 海宁市丁桥镇永畅知识产权服务部 | The preparation method of high temperature resistant aluminium paste glass powder |
CN115557706A (en) * | 2022-09-24 | 2023-01-03 | 江苏拜富科技股份有限公司 | Preparation process of high-performance glass powder |
CN115557706B (en) * | 2022-09-24 | 2024-04-12 | 江苏拜富科技股份有限公司 | Preparation process of high-performance glass powder |
CN116119934A (en) * | 2023-02-22 | 2023-05-16 | 江苏虹普电子材料科技有限公司 | NTC thermistor coated glass powder and preparation method thereof |
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