CN105060722B - Nano glass powder and preparation method thereof - Google Patents
Nano glass powder and preparation method thereof Download PDFInfo
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- CN105060722B CN105060722B CN201510584973.9A CN201510584973A CN105060722B CN 105060722 B CN105060722 B CN 105060722B CN 201510584973 A CN201510584973 A CN 201510584973A CN 105060722 B CN105060722 B CN 105060722B
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Abstract
The preparation method of the nano glass powder comprises the following steps: (1) Uniformly mixing a plurality of glass raw materials to form a mixed glass raw material, wherein the glass raw material comprises one or more of a non-metal oxide, an alkaline earth metal oxide or an alkali metal oxide; (2) Melting the mixed glass raw material to form a glass liquid; (3) Water quenching the glass liquid with a water quenching liquid in a highly turbulent state, thereby forming a glass suspension; and (4) drying and collecting the glass suspension, thereby obtaining the nano glass powder. Compared with the traditional preparation process, the preparation method has the advantages of short process and high yield, and the prepared nano glass powder has high purity, small particle size, uniform particle size distribution and good dispersibility, and can be applied to conductive slurry in the fields of microelectronics and solar cells.
Description
Technical Field
The invention relates to the field of inorganic nonmetallic materials, relates to nanometer glass powder, and in particular relates to a preparation process of the nanometer glass powder.
Background
The electronic paste is a base material of solar cells and microelectronic packages, is regarded as a key material of component packaging, electrodes and interconnection, is widely applied in the characteristics of high quality, high benefit, advanced technology, wide application and the like, and is a high-technology electronic functional material integrating chemical industry, electronic technology and metallurgy.
Electronic paste generally consists of three parts, namely a functional phase, a binding phase and an organic carrier. The functional phase mainly plays a role in conducting electricity, and the superfine glass powder and the organic carrier are used as binding phases and are uniformly dispersed in the organic carrier. At present, in the process of solar cell production and microelectronic packaging, electronic paste is generally transferred onto a cell or a circuit substrate by a screen printing technology, and conductive grid lines are formed by sintering and attached to a substrate. With the continuous progress of screen printing technology, the electrode wires of screen printing can reach a very fine degree, but in recent two years, a technology of an inkjet printing process is gradually developed, and the metal 'ink' used in the inkjet printing process is much more conductive than the conductive paste used in the screen printing process, and the inkjet printing process is also more accurate. Compared with the screen printing process, the metal wire width reaches 80-120 mu m, the wire width prepared by the novel process is much narrower and is only 30-40 mu m, so that the consumption of conductive paste can be reduced, and the cost is reduced. At the same time, narrower wires and better conductivity can also improve the photoelectric conversion efficiency of the solar cell, reduce the volume of the microelectronic device and improve the efficiency.
In the case of ink jet printing, the diameter of the nozzle of the ink jet head is in the range of 10 to 60 μm, and in order to avoid the occurrence of clogging during the ink jet printing, the particles of the substances in the ink must be strictly limited, so that the metal powder, glass frit and organic carrier particles in the ink are as low as 1 μm as possible. Meanwhile, in order to avoid precipitation of particles in the ink, it is actually required that the particle diameters of the metal powder and the frit be less than 100nm. At present, the technology for preparing nano metal powder is relatively mature, but for glass frit, the industrialized preparation of nano glass powder has a certain difficulty, and is one of the most critical technologies for ink-jet printing.
At present, three approaches are mainly adopted for preparing the glass powder for the electronic paste, namely a high-temperature melting method, a spray thermal decomposition method and a sol-gel method. The high-temperature melting method is characterized in that glass raw materials are uniformly mixed according to a certain metering ratio and then heated and melted, the glass raw materials are rapidly cooled to form glass frit, or water is quenched to form glass slag, and then the glass frit or the glass slag is crushed and ball-milled to obtain superfine glass powder. However, the method is not easy to prepare nano-scale glass powder, the composition of the glass can be changed by long-time ball milling, and impurities are introduced; the preparation of superfine glass powder by spray pyrolysis is an emerging preparation mode at present, and the method is to prepare the glass powder by micro-reaction of liquid drops, so that the glass powder is relatively uniform in size and composition, spherical in shape and good in dispersibility. The spray pyrolysis method is suitable for large-scale industrial production, but has high equipment requirement and high production cost; the superfine glass powder prepared by the sol-gel method is generally homogeneous and high-purity, the proportion of the components is well controlled, the preparation temperature is much lower than that of the traditional method, and the superfine glass powder has a certain rheological property. However, the method generally adopts metal alkoxide as a precursor, has high raw material cost and long reaction time, and is easy to remain carbon.
Disclosure of Invention
The invention aims to provide a nano glass powder and a preparation process thereof, which are improvements of the traditional high-temperature melting method.
In order to achieve the above object, there is provided a method for preparing nano glass powder, comprising the steps of (1) uniformly mixing a plurality of glass raw materials to form a mixed glass raw material, wherein the glass raw material comprises one or more of a non-metal oxide, an alkaline earth metal oxide, or an alkali metal oxide; (2) Melting the mixed glass raw material to form a glass liquid; (3) Water quenching the glass liquid with a water quenching liquid in a highly turbulent state, thereby forming a glass suspension; and (4) drying and collecting the glass suspension, thereby obtaining the nano glass powder.
In some embodiments, the non-metal oxide comprises SiO 2 ，B 2 O 3 ，Bi 2 O 3 。
In some embodiments, the alkaline earth metal oxide comprises BaO or CaO.
In some embodiments, the alkali metal oxide comprises Li 2 O，Na 2 O, or K 2 O。
In some embodiments, the mixed glass raw materials are placed in a high temperature furnace tunnel, warmed to 1400-1600 ℃ and held for 3-5 hours, thereby forming the glass liquid.
In some embodiments, deionized water is used for the water quenching, and polyethylene glycol is added in an amount of 0.1-0.5% by mass, thereby forming a water quenching liquid.
In some embodiments, a high shear disperser is used to place the water quench liquid in a highly turbulent state and to allow the glass liquid to evenly flow into the water quench liquid for quenching and rapid dispersion, thereby forming a glass suspension.
In some embodiments, the glass suspension is pumped into a centrifugal spray drying tower for drying and collection.
Compared with the traditional preparation process, the nano glass powder prepared by the method has the advantages of short process and high yield, and the prepared nano glass powder has high purity, small particle size, uniform particle size distribution and good dispersibility, and can be applied to conductive slurry in the fields of microelectronics and solar cells.
Other aspects and advantages of the invention will become apparent from the following description, taken in conjunction with the accompanying drawings, illustrating by way of example the principles of the invention.
Drawings
The above and other features and advantages of the present invention will be more clearly understood from the following detailed description taken in conjunction with the accompanying drawings, in which:
FIG. 1 is a process flow diagram of a method of preparing a nano-glass powder according to an embodiment of the invention;
fig. 2 to 3 are SEM images of the synthesis of nano glass powder under different process conditions in the specific example.
Detailed Description
The invention will be described in more detail hereinafter with reference to the drawings of specific embodiments of the invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.
The method for preparing the nano ceramic powder according to the embodiment of the invention will now be described in detail with reference to the accompanying drawings.
As shown in fig. 1, in step S101, a plurality of glass raw materials are uniformly mixed to form a mixed glass raw material, wherein the glass raw material includes one or more of a non-metal oxide, an alkaline earth metal oxide, or an alkali metal oxide.
In some embodiments, the non-metal oxide comprises SiO 2 ，B 2 O 3 ，Bi 2 O 3 . The alkaline earth metal oxide includes BaO or CaO. The alkali metal oxide comprises Li 2 O，Na 2 O, or K 2 O。
In step S102, the mixed glass raw material is melted to form a molten glass. In some embodiments, the mixed glass raw materials are placed in a high-temperature melting furnace channel, heated to 1400-1600 ℃ and kept for 3-5 hours, so as to form the glass melt;
in step S103, the glass liquid is water quenched with a water-floating liquid in a highly turbulent state, thereby forming a glass suspension. Deionized water is used for water quenching, and polyethylene glycol with the mass fraction of 0.1-0.5% is added, so that water quenching liquid is formed. The water quench liquid is placed in a highly turbulent state using a high shear disperser and the glass liquid is allowed to flow evenly into the water quench liquid for quenching and rapid dispersion, thereby forming a glass suspension.
In step S104, the glass suspension is dried and collected, thereby obtaining the nano glass powder. The glass suspension is pumped into a centrifugal spray drying tower for drying and collection.
The invention is further illustrated and described below in connection with specific embodiments.
Example 1
Weighing 20kg of glass frit SiO2 in 40% by mass percent; 20% of B2O 3; 5% of Bi2O 3; 20% of BaO; li (Li) 2 O:10％；Na 2 5% of O; after being evenly mixed, the mixture is placed in a corundum channel, the temperature is raised to 1580 ℃, and the heat is preserved for 3 hours.
Injecting 800L deionized water into a 1000L water quenching tank, and adding 50g of polyethylene glycol with molecular weight of 2000; starting the high-shear dispersing machine, wherein the rotating speed of a motor is 12000r/min, slowly opening a two-way flashboard, and slowly flowing glass liquid into a water floatation tank; after 30min, the high shear disperser was turned off to form a white glass suspension.
Starting a draught fan, an air filter, a blower and an air preheater in the spray drying unit, and enabling hot air to enter a drying tower uniformly in a spiral manner; starting a material pump, spraying glass material liquid through a tower top spray head (a high-speed centrifugal atomizer) and contacting with hot air; setting the inlet temperature of hot air to be 200 ℃, the outlet temperature to be 90 ℃ and the feeding speed of a material pump to be 1kg/min; under the action of an induced draft fan, the dried glass powder is collected at the bottom of the drying tower, at the bottom of the cyclone separator and in the bag-type dust collector; the average particle diameter of the obtained glass powder is 60nm.
An SEM image of the nano-glass powder of the formed glass powder is shown in fig. 2.
Example 2
Weighing 20kg of glass frit according to the following mass percentage: siO (SiO) 2 ：55％；B 2 O 3 ：15％；Bi 2 O 3 ：2.5％；CaO:15％；Li 2 O：7.5％；K 2 O:5%; after being evenly mixed, the mixture is placed in a corundum channel, the temperature is raised to 1600 ℃, and the heat is preserved for 4 hours.
Injecting 800L deionized water into a 1000L water quenching tank, and adding 40g of polyethylene glycol with molecular weight of 2000; starting the high-shear dispersing machine, wherein the rotating speed of a motor is 8000r/min, slowly opening a two-way flashboard, and slowly flowing glass liquid into a water floatation tank; after 60min, the high shear disperser was turned off to form a white glass suspension.
Starting a draught fan, an air filter, a blower and an air preheater in the spray drying unit, and enabling hot air to enter a drying tower uniformly in a spiral manner; starting a material pump, spraying glass material liquid through a tower top spray head (a high-speed centrifugal atomizer) and contacting with hot air; setting the inlet temperature of hot air to 200 ℃, the outlet temperature to 90 ℃ and the feeding speed of a material pump to 1.5kg/min; under the action of an induced draft fan, the dried glass powder is collected at the bottom of the drying tower, at the bottom of the cyclone separator and in the bag-type dust collector; the average particle diameter of the obtained glass powder is 90nm.
An SEM image of the nano-glass powder of the formed glass powder is shown in fig. 3.
Compared with the traditional preparation process, the preparation method has the advantages of short process and high yield, and the prepared nano glass powder has high purity, small particle size, uniform particle size distribution and good dispersibility, and can be applied to conductive slurry in the fields of microelectronics and solar cells.
The foregoing describes in detail preferred embodiments of the present invention. It should be understood that numerous modifications and variations can be made in accordance with the concepts of the invention by one of ordinary skill in the art without undue burden. The technical solutions which can be obtained by a person skilled in the art through logic analysis, reasoning or limited experiments based on the prior art according to the inventive concept shall be within the scope of protection defined by the claims.
Claims (5)
1. The preparation method of the nano glass powder is characterized by comprising the following steps:
(1) Uniformly mixing a plurality of glass raw materials to form a mixed glass raw material, wherein the glass raw material comprises nonmetal oxygen
One or more of a compound, an alkaline earth metal oxide, or an alkali metal oxide;
(2) Melting the mixed glass raw material to form a glass liquid;
(3) Water quenching the glass liquid with a water quenching liquid in a highly turbulent state, thereby forming a glass suspension; a kind of electronic device with high-pressure air-conditioning system
(4) Drying and collecting the glass suspension, thereby obtaining the nano glass powder;
in the step (3), deionized water is used for water quenching, and polyethylene glycol with the mass fraction of 0.1-0.5% is added, so that water quenching liquid is formed;
in step (3), using a high shear disperser to bring the water quenching liquid into a highly turbulent state and to allow the glass liquid to uniformly flow into the water quenching liquid for quenching and rapid dispersion, thereby forming a glass suspension;
in step (3), pumping the glass suspension into a centrifugal spray drying tower for drying and collection;
the diameter range of the nano glass powder is 50-100 nm;
the motor speed of the high-shear dispersing machine is 12000r/min or 8000r/min.
2. The method of claim 1, wherein in step (1), the non-metal oxide comprises SiO 2 ，B 2 O 3 。
3. The method of preparing nano glass powder according to claim 1, wherein in the step (1), the alkaline earth metal oxide comprises BaO or CaO.
4. The method for producing a nano-glass powder according to claim 1, wherein in the step (1), the alkali metal
The metal oxide includes Li 2 O，Na 2 O, or K 2 O。
5. The method of preparing nano glass powder according to claim 1, wherein in the step (2), the mixed glass raw material is placed in a high temperature melting furnace channel, heated to 1400-1600 ℃ and kept for 3-5 hours, thereby forming the glass liquid.
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| CN107555766B (en) * | 2017-09-06 | 2019-08-23 | 安徽凯盛基础材料科技有限公司 | Utilize the method for glass microballoon production solid phase converter |
| CN109036753B (en) * | 2018-07-02 | 2020-06-12 | 四川大学 | Amorphous nanocrystalline composite magnetic powder core and preparation method thereof |
| CN112851126B (en) * | 2021-03-19 | 2022-08-05 | 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 |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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