CN105060722A - Nano glass powder and preparation method thereof - Google Patents
Nano glass powder and preparation method thereof Download PDFInfo
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- CN105060722A CN105060722A CN201510584973.9A CN201510584973A CN105060722A CN 105060722 A CN105060722 A CN 105060722A CN 201510584973 A CN201510584973 A CN 201510584973A CN 105060722 A CN105060722 A CN 105060722A
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Abstract
The invention discloses a preparation method of nano glass powder. The preparation method comprises the following steps of firstly, uniformly mixing multiple kinds of glass raw materials to form a mixed glass raw material, wherein the glass raw materials comprise one or several kinds of nonmetallic oxides, alkaline earth metal oxides or alkali metal oxides; secondly, melting the mixed glass raw material to form liquid glass; thirdly, performing water quenching on the liquid glass by using a water quenching liquid in a highly turbulent state to form a glass suspension; fourthly, drying and collecting the glass suspension to obtain the nano glass powder. According to the preparation method disclosed by the invention, the nano glass powder is prepared by using a method of water quenching, high cut disperse and centrifugal spray drying; compared with a traditional preparation process, the preparation method has the advantages of short preparation process and high yield; the prepared nano glass powder is high in purity, small in particle size, uniform in particle size distribution and good in dispersion, and can be applied to conductive slurry in the fields of microelectronics and solar cells.
Description
Technical field
The present invention relates to field of inorganic nonmetallic material, relate to a kind of nano-glass powder, particularly relate to a kind of preparation technology of nano-glass powder.
Background technology
Electric slurry is the base mateiral of solar cell, microelectronics Packaging, be regarded as parts encapsulation, electrode and interconnected critical material, with high quality, high benefit, advanced technology, being suitable for the feature such as wide and being used widely, is integrate chemical industry, electronic technology, metallurgical a kind of high-tech electronics functional materials.
Electric slurry generally by function phase, Binder Phase and organic carrier three part form.Function mainly plays electric action mutually, and superfine glass powder, organic carrier are as Binder Phase, and they are dispersed in organic carrier uniformly.At present in manufacture of solar cells, microelectronics Packaging process, electric slurry is generally transfer on battery or circuit substrate by the technology of silk screen printing by electric slurry, forms conduction grid line be attached in substrate by sintering.Along with screen printing technique constantly progress, the electrode wires of silk screen printing can reach very tiny degree, but over the past two years, develop a kind of technology of InkJet printing processes gradually, the electrocondution slurry electroconductibility that the metal " ink " that InkJet printing processes uses uses than silk-screen printing technique is a lot of by force, and InkJet printing processes is also more accurate.Reach 80 ~ 120 μm relative to silk-screen printing technique metal guide live width, conductor width prepared by novel process is much narrow, is only 30 ~ 40 μm, certainly will can reduce the consumption of electrocondution slurry, reduces cost.Meanwhile, narrower wire, better electroconductibility also can improve the electricity conversion of solar cell, reduce the volume of microelectronic device and improve usefulness.
For ink jet printing, the diameter range of inkjet nozzle is at 10 ~ 60 μm, in ink jet printing process, there is the situation of plug, strictly must limit the particle of material in ink, make the metal-powder in ink, frit and organic carrier particle lower than 1 μm as far as possible.Meanwhile, in order to avoid the solids precipitation in ink, the particle diameter of actual requirement metal-powder and frit is less than 100nm.Prepare the technology relative maturity of nano metal powder at present, but for frit, preparation of industrialization goes out nano level glass powder and also has certain difficulty, is one of technology of spray ink Printing most critical.
Prepare electric slurry glass powder at present and mainly contain three approach: high-temperature melting method, spray heating decomposition, sol-gel method.High-temperature melting method frit is mixed post-heating by certain metering ratio melt, quick cooling forms glass frit, or shrend becomes glass dregs, then by glass frit or glass dregs is broken, ball milling obtains palladium powder, the method prepares simple and fast, and output is large.But the method not easily prepares the glass powder of Nano grade, long-time ball milling also may change the composition of glass, introduces impurity; It is preparation method emerging at present that spray-wall interaction mode prepares palladium powder, and the method prepares glass powder by micro-reaction of drop, relatively uniform in size and component, presents spherical, better dispersed.Spray heating decomposition is applicable to large-scale industrial production, but high to equipment requirements, and production cost is high; The general homogeneous of palladium powder prepared by sol-gel method is high-purity, and moiety proportioning better controls, and preparation temperature is compared much lower with traditional method, have certain rheological properties.But the method generally adopts metal alkoxide as precursor, and raw materials cost is high, reaction times longer and easy residual charcoal.
Summary of the invention
The present invention aims to provide a kind of for solving the problem, and the present invention proposes a kind of nano-glass powder and preparation technology thereof, is improve the one of conventional high-temperature scorification.
In order to reach above-mentioned purpose, provide a kind of preparation method of nano-glass powder, comprise the steps: that multiple frit mixes to form hybrid glass raw material by (1), wherein said frit comprises nonmetal oxide, alkaline earth metal oxide, or one or more in alkalimetal oxide; (2) make described hybrid glass raw materials melt and form glass metal; (3) use the shrend liquid being in high turbulence state to carry out shrend to described glass metal, thus form glass suspension; And (4) carry out drying and collection to described glass suspension, thus obtain described nano-glass powder.
In some embodiments, described nonmetal oxide comprises SiO
2, B
2o
3, Bi
2o
3.
In some embodiments, described alkaline earth metal oxide comprises BaO or CaO.
In some embodiments, described alkalimetal oxide comprises Li
2o, Na
2o, or K
2o.
In some embodiments, described hybrid glass raw material is placed in high-temperature smelting pot passage, is warming up to 1400 ~ 1600 DEG C and is incubated 3 ~ 5h, thus form described glass metal.
In some embodiments, described shrend uses deionized water, and adds the polyoxyethylene glycol that massfraction is 0.1 ~ 0.5%, thus forms shrend liquid.
In some embodiments, use high-shear dispersion machine to make described shrend liquid be in the state of high turbulence, and make described glass metal evenly flow into described shrend liquid to carry out chilling and be quickly dispersed out, thus form glass suspension.
In some embodiments, described glass suspension is pumped in centrifugal spray drying tower to carry out drying and collection.
The present invention adopts the method for shrend-high-shear dispersion-centrifugal spray drying to prepare described nano-glass powder, compared with traditional preparation technology, there is the advantage that processing procedure is short, productive rate is high, the nano-glass powder purity prepared is high, particle diameter is little, even particle size distribution, good dispersity, can be applicable to microelectronics and area of solar cell electrocondution slurry.
Below in conjunction with accompanying drawing, the description of purport of the present invention is described by example, to know other aspects of the present invention and advantage.
Accompanying drawing explanation
By reference to the accompanying drawings, by detailed description hereafter, above-mentioned and other feature and advantage of the present invention more clearly can be understood, wherein:
Fig. 1 is the process flow sheet of the preparation method of barium calcium silicon system composite nano-ceramic powder according to the embodiment of the present invention;
Fig. 2 ~ Fig. 5 is the SEM figure of different technology conditions synthesis barium calcium silicon system composite nano-ceramic powder in specific embodiment.
Embodiment
See the accompanying drawing of the specific embodiment of the invention, hereafter in more detail the present invention will be described.But the present invention can realize in many different forms, and should not be construed as by the restriction in the embodiment of this proposition.On the contrary, it is abundant and complete open in order to reach for proposing these embodiments, and makes those skilled in the art understand scope of the present invention completely.
Description describes the preparation method according to the nano-ceramic powder of the embodiment of the present invention in detail.
As described in Figure 1, according to the preparation method of the nano-glass powder of the embodiment of the present invention, in step S101, multiple frit is mixed to form hybrid glass raw material, wherein said frit comprises nonmetal oxide, alkaline earth metal oxide, or one or more in alkalimetal oxide.
In some embodiments, described nonmetal oxide comprises SiO
2, B
2o
3, Bi
2o
3.described alkaline earth metal oxide comprises BaO or CaO.Described alkalimetal oxide comprises Li
2o, Na
2o, or K
2o.
In step S102, make described hybrid glass raw materials melt and form glass metal.In some embodiments, described hybrid glass raw material is placed in high-temperature smelting pot passage, is warming up to 1400 ~ 1600 DEG C and is incubated 3 ~ 5h, thus form described glass melt;
In step S103, use the shrend liquid being in high turbulence state to carry out shrend to described glass metal, thus form glass suspension.Described shrend uses deionized water, and adds the polyoxyethylene glycol that massfraction is 0.1 ~ 0.5%, thus forms shrend liquid.Use high-shear dispersion machine to make described shrend liquid be in the state of high turbulence, and make described glass metal evenly flow into described shrend liquid to carry out chilling and be quickly dispersed out, thus form glass suspension.
In step S104, drying and collection are carried out to described glass suspension, thus obtain described nano-glass powder.Described glass suspension is pumped in centrifugal spray drying tower to carry out drying and collection.
Below in conjunction with specific embodiment, the invention will be further elaborated.
Embodiment 1
20kg frit is taken: SiO by following mass percent
2: 40%; B
2o
3: 20%; Bi
2o
3: 5%; BaO:20%; Li
2o:10%; Na
2o:5%; Mix and be placed in corundum passage, be warming up to 1580 DEG C, insulation 3h.
Inject 800L deionized water in 1000L water quenching pool, add the polyoxyethylene glycol 50g of molecular weight 2000; Open high-shear dispersion machine, motor speed is 12000r/min, slowly opens bidirectional flashboard, and glass metal slowly flows in water quenching pool; After 30min, close high-shear dispersion machine and form white glass suspension.
Open induced draft fan, air filter, fan and the air preheater in spraying dry unit, warm air enters drying tower in the shape of a spiral equably; Open material pump, glass feed liquid sprays, with hot air through tower top shower nozzle (high speed centrifugal atomization device); Setting hot air inlet temperature is 200 DEG C, and temperature out is 90 DEG C, and material pump delivery rate is 1kg/min; Under the effect of induced draft fan, dried glass powder is collected at the bottom of drying tower, bottom cyclonic separator and in sack cleaner; Gained glass powder Electronic Speculum median size is 60nm.
The SEM figure of the nano-glass powder of the glass powder formed as shown in Figure 2.
Embodiment 2
20kg frit is taken: SiO by following mass percent
2: 55%; B
2o
3: 15%; Bi
2o
3: 2.5%; CaO:15%; Li
2o:7.5%; K
2o:5%; Mix and be placed in corundum passage, be warming up to 1600 DEG C, insulation 4h.
Inject 800L deionized water in 1000L water quenching pool, add the polyoxyethylene glycol 40g of molecular weight 2000; Open high-shear dispersion machine, motor speed is 8000r/min, slowly opens bidirectional flashboard, and glass metal slowly flows in water quenching pool; After 60min, close high-shear dispersion machine and form white glass suspension.
Open induced draft fan, air filter, fan and the air preheater in spraying dry unit, warm air enters drying tower in the shape of a spiral equably; Open material pump, glass feed liquid sprays, with hot air through tower top shower nozzle (high speed centrifugal atomization device); Setting hot air inlet temperature is 200 DEG C, and temperature out is 90 DEG C, and material pump delivery rate is 1.5kg/min; Under the effect of induced draft fan, dried glass powder is collected bottom drying tower, bottom cyclonic separator and in sack cleaner; Gained glass powder Electronic Speculum median size is 90nm.
The SEM figure of the nano-glass powder of the glass powder formed as shown in Figure 3.
The present invention adopts the method for shrend-high-shear dispersion-centrifugal spray drying to prepare described nano-glass powder, compared with traditional preparation technology, there is the advantage that processing procedure is short, productive rate is high, the nano-glass powder purity prepared is high, particle diameter is little, even particle size distribution, good dispersity, can be applicable to microelectronics and area of solar cell electrocondution slurry.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that those of ordinary skill in the art just design according to the present invention can make many modifications and variations without the need to creative work.All technician in the art, all should by the determined protection domain of claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (10)
1. a preparation method for nano-glass powder, is characterized in that, comprises the steps:
(1) mixed to form hybrid glass raw material by multiple frit, wherein said frit comprises nonmetal oxide, alkaline earth metal oxide, or one or more in alkalimetal oxide;
(2) make described hybrid glass raw materials melt and form glass metal;
(3) use the shrend liquid being in high turbulence state to carry out shrend to described glass metal, thus form glass suspension; And
(4) drying and collection are carried out to described glass suspension, thus obtain described nano-glass powder.
2. the preparation method of nano-glass powder according to claim 1, is characterized in that, in step (1), described nonmetal oxide comprises SiO
2, B
2o
3, Bi
2o
3.
3. the preparation method of nano-glass powder according to claim 2, is characterized in that, in step (1), described alkaline earth metal oxide comprises BaO or CaO.
4. the preparation method of nano-glass powder according to claim 3, is characterized in that, in step (1), described alkalimetal oxide comprises Li
2o, Na
2o, or K
2o.
5. the preparation method of nano-glass powder according to claim 1, it is characterized in that, in step (2), described hybrid glass raw material is placed in high-temperature smelting pot passage, be warming up to 1400 ~ 1600 DEG C and be incubated 3 ~ 5h, thus forming described glass metal.
6. the preparation method of nano-glass powder according to claim 1, is characterized in that, in step (3), described shrend uses deionized water, and adds the polyoxyethylene glycol that massfraction is 0.1 ~ 0.5%, thus forms shrend liquid.
7. the preparation method of nano-glass powder according to claim 5, it is characterized in that, in step (3), high-shear dispersion machine is used to make described shrend liquid be in the state of high turbulence, and make described glass metal evenly flow into described shrend liquid carry out chilling and be quickly dispersed out, thus form glass suspension.
8. the preparation method of nano-glass powder according to claim 1, is characterized in that, in step (3), is pumped into by described glass suspension in centrifugal spray drying tower to carry out drying and collection.
9. a nano-glass powder, is characterized in that, described glass powder is made up of nonmetal oxide and metal oxide, and its particle size range is 50 ~ 100nm.
10. nano-glass powder as claimed in claim 9, it is characterized in that, this glass powder comprises following component: SiO
2, 30 ~ 60% mass percents, B
2o
3, 0 ~ 20% mass percent, Bi
2o
3, 0 ~ 5% mass percent, BaO, 0 ~ 30% mass percent, or CaO, 0 ~ 30% mass percent.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107555766A (en) * | 2017-09-06 | 2018-01-09 | 安徽凯盛基础材料科技有限公司 | The method that solid phase converter is made using glass microballoon |
| CN109036753A (en) * | 2018-07-02 | 2018-12-18 | 四川大学 | A kind of amorphous nano-crystalline composite magnetic powder core and preparation method thereof |
| CN112851126A (en) * | 2021-03-19 | 2021-05-28 | 厦门Abb 避雷器有限公司 | Lead-free composite glass powder for insulating side surface of ZnO resistance card, preparation method and glass glaze |
| CN114751647A (en) * | 2022-03-29 | 2022-07-15 | 华南理工大学 | Glass frit easy to grind and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003212572A (en) * | 2002-01-18 | 2003-07-30 | Hitachi Metals Ltd | Method of manufacturing spherical glass powder |
| CN101094818A (en) * | 2004-05-29 | 2007-12-26 | 肖特股份公司 | Nano glass powder and use thereof, particularly multicomponent glass powder with a mean particle size of less than 1 [mu]m |
| US20140243185A1 (en) * | 2011-10-20 | 2014-08-28 | Inha-Industry Partnership Institute | Method and apparatus for manufacturing a low melting point nano glass powder |
-
2015
- 2015-09-15 CN CN201510584973.9A patent/CN105060722B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003212572A (en) * | 2002-01-18 | 2003-07-30 | Hitachi Metals Ltd | Method of manufacturing spherical glass powder |
| CN101094818A (en) * | 2004-05-29 | 2007-12-26 | 肖特股份公司 | Nano glass powder and use thereof, particularly multicomponent glass powder with a mean particle size of less than 1 [mu]m |
| US20140243185A1 (en) * | 2011-10-20 | 2014-08-28 | Inha-Industry Partnership Institute | Method and apparatus for manufacturing a low melting point nano glass powder |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107555766A (en) * | 2017-09-06 | 2018-01-09 | 安徽凯盛基础材料科技有限公司 | The method that solid phase converter is made using glass microballoon |
| CN109036753A (en) * | 2018-07-02 | 2018-12-18 | 四川大学 | A kind of amorphous nano-crystalline composite magnetic powder core and preparation method thereof |
| CN112851126A (en) * | 2021-03-19 | 2021-05-28 | 厦门Abb 避雷器有限公司 | Lead-free composite glass powder for insulating side surface of ZnO resistance card, preparation method and glass glaze |
| CN114751647A (en) * | 2022-03-29 | 2022-07-15 | 华南理工大学 | Glass frit easy to grind and preparation method and application thereof |
| CN114751647B (en) * | 2022-03-29 | 2023-06-20 | 华南理工大学 | Glass frit easy to grind and preparation method and application thereof |
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| CN105060722B (en) | 2023-07-07 |
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