CN108010602A - A kind of preparation process of Nano glass powder - Google Patents
A kind of preparation process of Nano glass powder Download PDFInfo
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- CN108010602A CN108010602A CN201711229802.XA CN201711229802A CN108010602A CN 108010602 A CN108010602 A CN 108010602A CN 201711229802 A CN201711229802 A CN 201711229802A CN 108010602 A CN108010602 A CN 108010602A
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- glass powder
- preparation process
- nano
- nano glass
- dispersant
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- 239000011521 glass Substances 0.000 title claims abstract description 79
- 239000000843 powder Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000002270 dispersing agent Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 21
- 238000000227 grinding Methods 0.000 claims description 38
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 32
- 229910052726 zirconium Inorganic materials 0.000 claims description 32
- 239000000428 dust Substances 0.000 claims description 25
- 239000000725 suspension Substances 0.000 claims description 18
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 16
- 239000002994 raw material Substances 0.000 claims description 14
- 229920001577 copolymer Polymers 0.000 claims description 13
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N dimethylmethane Natural products CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000002904 solvent Substances 0.000 claims description 13
- 239000003607 modifier Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 239000001294 propane Substances 0.000 claims description 8
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- 238000013329 compounding Methods 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 4
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 4
- 229920001897 terpolymer Polymers 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- 229920002125 Sokalan® Polymers 0.000 claims description 3
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 claims description 3
- 239000004584 polyacrylic acid Substances 0.000 claims description 3
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 3
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 3
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 3
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 229940028356 diethylene glycol monobutyl ether Drugs 0.000 claims description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 2
- 239000011976 maleic acid Substances 0.000 claims description 2
- JCGNDDUYTRNOFT-UHFFFAOYSA-N oxolane-2,4-dione Chemical compound O=C1COC(=O)C1 JCGNDDUYTRNOFT-UHFFFAOYSA-N 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 2
- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 12
- 238000007641 inkjet printing Methods 0.000 abstract description 10
- 239000006185 dispersion Substances 0.000 abstract description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 abstract description 2
- 238000000713 high-energy ball milling Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 9
- 239000002002 slurry Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000002844 melting Methods 0.000 description 4
- 230000008018 melting Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- KCXFHTAICRTXLI-UHFFFAOYSA-N propane-1-sulfonic acid Chemical compound CCCS(O)(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-N 0.000 description 3
- 238000004062 sedimentation Methods 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- 229910019142 PO4 Inorganic materials 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 125000003368 amide group Chemical group 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 230000000903 blocking effect Effects 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- 238000003921 particle size analysis Methods 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 238000010248 power generation Methods 0.000 description 2
- 238000007639 printing Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000007650 screen-printing Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- -1 sulphonic acid ester Chemical class 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 125000003903 2-propenyl group Chemical group [H]C([*])([H])C([H])=C([H])[H] 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 150000001412 amines Chemical group 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000010316 high energy milling Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 125000004464 hydroxyphenyl group Chemical group 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 230000010534 mechanism of action Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 239000011297 pine tar Substances 0.000 description 1
- 229940068124 pine tar Drugs 0.000 description 1
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 210000000498 stratum granulosum Anatomy 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/02—Details
- H01L31/0224—Electrodes
- H01L31/022408—Electrodes for devices characterised by at least one potential jump barrier or surface barrier
- H01L31/022425—Electrodes for devices characterised by at least one potential jump barrier or surface barrier for solar cells
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
Abstract
The present invention relates to a kind of preparation process of Nano glass powder, dispersant is coordinated to prepare Nano glass powder by high-energy ball milling method, average grain diameter is in 60~120nm, and not free settling, reunion, it can be scattered in nano silver conductive ink, the inkjet printing for solar cel electrode.Compared with prior art, nano-glass powder purity height that the present invention prepares, epigranular, particle diameter is small, technique is simple, solve the problems, such as that nano-glass is mutually difficult to prepare in solar cell ink-jet printing ink, can finally be made the solar cel electrode ink-jet printing ink that good dispersion, stability are high, do not block nozzle.
Description
Technical field
The invention belongs to field of inorganic nonmetallic material, more particularly, to a kind of preparation process of Nano glass powder.
Background technology
Since eighties of last century oil crisis, each state all carrys out alleviating energy crisis in a kind of new energy of discussion.Solar-electricity
Sunlight is directly converted into electric power by pond, is a kind of clean energy resource, thus this novel energy increasingly receives much concern.With too
The lifting of positive energy cell photoelectric transfer efficiency, the cost of photovoltaic generation is sunny local close to thermal power generation cost, state
Border energy administration prediction solar power generation amount accounts for the 16% of global generated energy in the year two thousand fifty, will be the main shape of future source of energy acquisition
One of formula.
The preparation method of traditional solar cel electrode is silk-screen printing.In screen printing technique, the perforate about 30- of web plate
45 μm, after slurry single printing-sintering, width is even broader at 50~60 μm, and height is generally at 12~20 μm, its height and width
The ratio of degree has the possibility that electrode breaks below 0.4, and due to printing net hole plug.If using inkjet printing skill
Art, successively prints accumulation molding, be able to can be done with the thin grid line of 30-50 microns of formation width, 30-50 microns of height, depth-width ratio
To 1, shading-area can be reduced, electrode internal resistance is reduced and improves transfer efficiency, while also reduces silver paste consumption.It is molded
Mechanism is that ink jet-print head exists in ink jet printing to base material cell piece since base station heats reason cell piece surface temperature
150-200 DEG C, ink droplet is ejected into cell piece surface solvent and volatilizees rapidly, and remaining solid particle is accumulated on surface, repeatedly same
One local spray printing, grid line will progressively increase and line width remains unchanged.
For ink jet printing, the diameter range of inkjet nozzle is at 10~60 μm, in order to avoid in ink jet printing process
There is the situation of plug, it is necessary to the particle of material in ink is strictly limited, make as far as possible metal dust in ink, frit with
And organic carrier particle is less than 1 μm.Meanwhile in order to avoid the particle precipitation in ink, actual requirement metal dust and frit
Particle diameter be less than 200nm.The technology relative maturity of nano metal powder is prepared at present, but for frit, industrialization
Preparing nano level glass powder also has certain difficulty, is one of solar cel electrode inkjet printing key technology.
Preparing electric slurry glass dust mainly has three approach at present：High-temperature melting method, spray heating decomposition, colloidal sol-
Gel method.High-temperature melting method is to rapidly cool to form glass than heating and melting after mixing by certain metering by frit
Glass frit, or water quenching crush acquisition glass dust into glass dregs, then by glass frit or glass dregs, and this method prepares simple fast
Victory, yield are big.But this method is not easy to prepare the glass dust of Nano grade；Spray-wall interaction mode prepares palladium powder
It is preparation method emerging at present, this method is to prepare glass dust by micro- reaction of drop, opposite in size and component
Uniformly, presentation is spherical, and dispersiveness is preferably.Spray heating decomposition is adapted to large-scale industrial production, but high to equipment requirement, raw
Produce of high cost；The general homogeneous of palladium powder prepared by sol-gel process is high-purity, and constituent matches somebody with somebody relatively good control, prepares temperature
Degree is compared much lower with conventional method, has a certain rheological properties, but this method generally uses metal alkoxide as predecessor, raw material
Of high cost, the reaction time is longer and easily remains charcoal.
The Chinese invention patent that publication No. is CN102815870A discloses a kind of laser-resistance composite heating evaporation and prepares
The method of Nano glass powder；Publication No. be CN105060722A Chinese invention patent disclose a kind of water quenching-high shear dispersion-
The method that centrifugal spray prepares Nano glass powder.Both the above method is required for being handled again after glass dust is melted completely,
There are complex process, it is high to equipment requirement, energy consumption is big the shortcomings of, and easily introduce pollution in melting.Publication No. is
The Chinese invention patent of CN106082682A discloses a kind of method for preparing glass air brushing glass dust suspension, which does not have
Have using suitable dispersant, preparation process is up to 24-48h, and sedimentation, agglomeration necessarily occurs in obtained suspension.
The content of the invention
It is an object of the present invention to overcome the above-mentioned drawbacks of the prior art and provide a kind of Nano glass powder
Preparation process.
The purpose of the present invention can be achieved through the following technical solutions：
A kind of preparation process of Nano glass powder, using following steps：
(1) it is 1~10 by weight by glass dust raw material, solvent and corase grinding zirconium ball:1~10:10~50 ratio is mixed
Close, 30~120min is roughly ground under 200~500rpm；
(2) corase grinding zirconium ball is taken out, adds fine grinding zirconium ball, by glass dust raw material, solvent, fine grinding zirconium ball, scattered
Agent is 1~10 by weight:1~10:10~50:0.1~2 ratio mixing, 30~60min of fine grinding under 400~800rpm,
Zirconium ball is taken out, obtains Nano glass powder suspension.
The dispersant is formed by dispersant host agent and surface modifier compounding, and the dispersant host agent accounts for gross weight
80%-90%, the surface modifier accounts for the 10%-20% of gross weight.
The dispersant host agent for methylacryoyloxyethyl dimethyl amine (DM) -1,3- propane sultones copolymer,
3- (2- methylacryoyloxyethyls dimethylamino) propane sulfonic acid-methyl allyl polyoxyethylene ether copolymer, humic acid-pi-allyl
Sodium sulfonate-dimethyl diallyl ammonium chloride terpolymer, methyl methacrylate-horse industry acid anhydride copolymer or maleic acid
One or more in acid anhydride-butyl methacrylate-styrene copolymer.It is preferred that 3- (2- methacryls can be used
Oxygen ethyl dimethylamino) propane sulfonic acid-methyl allyl polyoxyethylene ether copolymer or maleic anhydride-methyl butyl acrylate-benzene
Ethylene-dien terpolymer.
The active group of peptizaiton is played in dispersant host agent mainly amido, quaternary amine base, sulfonic group, propane sulfonic acid base, third
It is several in sulphonic acid ester, acrylate, phosphate, carboxyl, hydroxy phenyl.
The mechanism of action of dispersant is：Carboxyl, sulfonic group, phosphate, hydroxyl, amido etc. or their compound and nanometer
Powder surface combines, there is provided repulsion after good hydrophilicity and electrostatic；In addition functional group such as propane sulfonic acid base, propane sulfonic acid
Ester, acrylate and linear or branched alkyl form Third monomer, can improve the steric hindrance of dispersant, further enhance point
The dispersion effect of powder.
The dispersant announced using this patent can substantially reduce the time that preparation process is consumed, and the nanometer glass prepared
Glass powder suspension is not susceptible to sedimentation, agglomeration.
The surface modifier is silane coupling agent, polyacrylic acid, OP-10,2- chloracrylic acid or polyvinylpyrrolidine
One or more in ketone.
The solvent be selected from water, ethanol, ethylene glycol, diethylene glycol monobutyl ether, ether, acetone, styrene, isopropanol or
One or more in terpinol.
The corase grinding is with the sphere diameter of zirconium ball in 3~20mm, and fine grinding is with the sphere diameter of zirconium ball in 0.5~3mm.On the one hand, grind
Spherolite footpath is bigger, bigger from the energy of ball transmission feed in each ball, material collision, is conducive to smashing for material, thus if
Directly ball milling is carried out using minor diameter ball, then having many frits can not be broken, so needing first to be carried out with larger ball
Preliminary grinding.On the other hand, since big sphere gap is larger, abrading-ball gap will be hidden in certain fineness glass powder, mechanical milling process without
Method continues, so being milled to nano-scale using small zirconium ball after frit is smashed.
Glass dust raw material：Solvent：Corase grinding uses zirconium ball=1~10:1~10:10~50, it is preferable that ratio of grinding media to material 10:1, Gu
Liquor ratio 1:0.8.Increase ratio of grinding media to material can increase the collision frequency of abrading-ball and glass dust, reduce the mean free path of abrading-ball, abrading-ball
Capturing the probability of powder granule is also increasing.The generation reunited can effectively be suppressed；If ratio of grinding media to material is excessive, with abrading-ball quantity
The probability that increase, abrading-ball itself collision and abrading-ball are collided with ball grinder also increases, very big to ball grinder and abrading-ball itself abrasion.Gu
When liquor ratio is low, the less of solid particle in slurry by the probability of pellet impact with regard to small, so low production efficiency；And high solid-liquid ratio meeting
Cause slurry Reynolds number ReReduction, so as to cause the impact force of slurry and shearing force to taper into, powder is formed between medium
Stratum granulosum so that the trend that granularity reduces slows down.
Corase grinding rotating speed is in 200~500rpm in step (1), and the time is in 30~120min；Fine grinding rotating speed 400 in step (2)
~800rpm, the time is in 30~60min.Time is longer, rotating speed is higher, and ball milling effect is better, but overlong time, rotating speed are excessive all
The raising of cost can be caused, so suitable rotating speed and time should be selected.
The average grain diameter of Nano glass powder is in 60~120nm in the Nano glass powder suspension, and has used self-control
Dispersant, soilless sticking, sedimentation phenomenon.Glass dust is ink-jet printing ink as the critical function phase in solar cel electrode
In be easy to cause the bottleneck material of nozzle blocking, therefore should try one's best and reduce its particle diameter and prevent from reuniting, in order to avoid plug nozzle.Separately
Outside, less particle diameter can reduce sintering temperature in the technique for be subsequently formed Ohmic contact, advantageously reduce solar cell effect
The loss of rate.
Compared with prior art, the present invention using high-energy-milling and has used homemade dispersant and prepares a nanometer glass
Glass powder, has the characteristics that technique is simple, time-consuming short, low for equipment requirements, and without glass powder is melted in preparation process,
Prevent the pollution that may be introduced and energy consumption can be reduced, preparation process green high-efficient.Homemade dispersant can greatly reduce ball
Consume time, and can effectively disperse Nano glass powder to prevent from reuniting and settle.Obtained Nano glass powder particle diameter is small, it is uniform,
Good dispersion, stability are strong, can efficiently solve the problem of blocking nozzle when inkjet printing prepares solar cel electrode.
Brief description of the drawings
Fig. 1 is the laser particle size analysis figure of obtained Nano glass powder suspension in embodiment 1；
Fig. 2 is the laser particle size analysis figure of obtained Nano glass powder suspension in embodiment 2.
Embodiment
With reference to specific embodiment, the present invention is described in detail.Following embodiments will be helpful to the technology of this area
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill to this area
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection domain.
Embodiment 1
100g glass dust raw materials, 200g10mm zirconiums ball, 100g dibutyl ethylene glycol ethers is taken to add in ball grinder, by cooling water
Circuit is opened, and is ground 50min under 300rpm, is gone out zirconium ball using 200 mesh sieve net filtrations.
Prepare 5g dispersants, specific method is：Take 2g methylacryoyloxyethyls dimethyl amine (DM) -1,3-N-morpholinopropanesulfonic acid
Lactone copolymers, 2g methyl methacrylates-horse industry acid anhydride copolymer, 0.5g polyacrylic acid, 0.5gOP-10, stir evenly.
Glass dust suspension after preliminary grinding is refunded into ball grinder, and adds 1000g3mm zirconiums ball and to add 5g ready
Dispersant.
80min is ground at 600 rpm, is taken out zirconium ball using 400 mesh sieve nets, and Nano glass powder suspension is made.
Grain size analysis is carried out to obtained Nano glass powder suspension using nanometer laser particle size analyzer, average grain diameter exists
101nm, specific granularity is as shown in table 1, and acquired results are as shown in Figure 1.
Table 1
Grain-size characteristic parameter
Embodiment 2
Take 100g glass dust raw materials, 200g7mm zirconiums ball, 100g ethanol to add in ball grinder, chilled(cooling) water return (CWR) opened,
60min is ground under 200rpm, goes out zirconium ball using 200 mesh sieve net filtrations.
Prepare 5g dispersants, specific method is：Take 4g 3- (2- methylacryoyloxyethyls dimethylamino) propane sulfonic acid-first
Base allyl polyethenoxy ether copolymer, 0.5g humic acid-Sodium Allyl Sulfonate-dimethyl two-allyl ammonium chloride ternarys
Copolymer, polyvinylpyrrolidone 0.5g, stir evenly.
Glass dust suspension after preliminary grinding is refunded into ball grinder, and adds 1000g1mm zirconiums ball and to add 5g ready
Dispersant.
60min is ground at 500 rpm, is taken out zirconium ball using 400 mesh sieve nets, and Nano glass powder suspension is made.
Grain size analysis is carried out to obtained Nano glass powder suspension using nanometer laser particle size analyzer, average grain diameter exists
109nm, specific granularity is as shown in table 2, and acquired results are as shown in Figure 2.
Table 2
Grain-size characteristic parameter
Embodiment 3
A kind of preparation process of Nano glass powder, using following steps：
(1) it is 1 by weight in 3mm corase grinding zirconiums ball by glass dust raw material, aqueous solvent and sphere diameter:1:10 ratio is mixed
Close, roughly grind 120min at 200 rpm；
(2) corase grinding zirconium ball is taken out, addition sphere diameter is 0.5mm fine grinding zirconium balls, by glass dust raw material, solvent, fine grinding
It is 1 by weight with zirconium ball, dispersant:1:10:0.1 ratio mixing, the fine grinding 60min under 400rpm, the dispersant used
By dispersant host agent methylacryoyloxyethyl dimethyl amine (DM) -1,3- propane sultones copolymer and surface modifier silane
Coupling agent compounding forms, and dispersant host agent accounts for the 80% of gross weight, and surface modifier accounts for the 20% of gross weight, then takes zirconium ball
Go out, obtain Nano glass powder suspension, wherein the average grain diameter of Nano glass powder is in 60nm.
Embodiment 4
A kind of preparation process of Nano glass powder, using following steps：
(1) it is 3 by weight in 10mm corase grinding zirconiums ball by glass dust raw material, pine tar alcoholic solvent and sphere diameter:7:40 ratio
Example mixing, roughly grinds 60min at 300 rpm；
(2) corase grinding zirconium ball is taken out, addition sphere diameter is 1mm fine grinding zirconium balls, and glass dust raw material, solvent, fine grinding are used
Zirconium ball, dispersant are 3 by weight:2:40:1 ratio mixes, at 600 rpm fine grinding 40min, and the dispersant used is by dividing
Powder host agent methyl methacrylate-horse industry acid anhydride copolymer and surface modifier OP-10 compoundings form, and dispersant host agent accounts for always
The 85% of weight, surface modifier account for the 15% of gross weight, then take out zirconium ball, obtain Nano glass powder suspension, wherein
The average grain diameter of Nano glass powder is in 100nm.
Embodiment 5
A kind of preparation process of Nano glass powder, using following steps：
(1) it is 10 by weight in 20mm corase grinding zirconiums ball by glass dust raw material, ether solvent and sphere diameter:10:50 ratio
Example mixing, roughly grinds 30min at 500 rpm；
(2) corase grinding zirconium ball is taken out, addition sphere diameter is 3mm fine grinding zirconium balls, and glass dust raw material, solvent, fine grinding are used
Zirconium ball, dispersant are 10 by weight:10:50:2 ratio mixing, fine grinding 40min at 600 rpm, the dispersant used by
Dispersant host agent maleic anhydride-methyl butyl acrylate-styrene terpolymer and surface modifier polyvinylpyrrolidone
Compounding forms, and dispersant host agent accounts for the 90% of gross weight, and surface modifier accounts for the 10% of gross weight, then takes out zirconium ball, obtains
To Nano glass powder suspension, wherein the average grain diameter of Nano glass powder is in 120nm.
The specific embodiment of the present invention is described above.It is to be appreciated that the invention is not limited in above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring the substantive content of the present invention.
Claims (9)
1. a kind of preparation process of Nano glass powder, it is characterised in that the technique uses following steps：
(1) it is 1~10 by weight by glass dust raw material, solvent and corase grinding zirconium ball:1~10:10~50 ratio mixing,
30~120min is roughly ground under 200~500rpm；
(2) corase grinding zirconium ball is taken out, adds fine grinding zirconium ball, glass dust raw material, solvent, fine grinding are pressed with zirconium ball, dispersant
Weight ratio is 1~10:1~10:10~50:0.1~2 ratio mixing, 30~60min of fine grinding under 400~800rpm, by zirconium
Ball takes out, and obtains Nano glass powder suspension.
2. the preparation process of a kind of Nano glass powder according to claim 1, it is characterised in that the dispersant is by dividing
Powder host agent and surface modifier compounding form, and the dispersant host agent accounts for the 80%-90% of gross weight, and the surface changes
Property agent accounts for the 10%-20% of gross weight.
A kind of 3. preparation process of Nano glass powder according to claim 2, it is characterised in that the dispersant host agent
For methylacryoyloxyethyl dimethyl amine (DM) -1,3- propane sultones copolymer, 3- (2- methylacryoyloxyethyl diformazans
Amino) propane sulfonic acid-methyl allyl polyoxyethylene ether copolymer, humic acid-Sodium Allyl Sulfonate-dimethyl diallyl chlorination
Ammonium terpolymer, methyl methacrylate-horse industry acid anhydride copolymer or maleic anhydride-methyl butyl acrylate-styrene three
One or more in membered copolymer.
A kind of 4. preparation process of Nano glass powder according to claim 2, it is characterised in that the dispersant host agent
Preferably 3- (2- methylacryoyloxyethyls dimethylamino) propane sulfonic acid-methyl allyl polyoxyethylene ether copolymers or maleic acid
Acid anhydride-butyl methacrylate-styrene copolymer.
A kind of 5. preparation process of Nano glass powder according to claim 2, it is characterised in that the surface modifier
For the one or more in silane coupling agent, polyacrylic acid, OP-10,2- chloracrylic acid or polyvinylpyrrolidone.
6. the preparation process of a kind of Nano glass powder according to claim 1, it is characterised in that the solvent is selected from
One or more in water, ethanol, ethylene glycol, diethylene glycol monobutyl ether, ether, acetone, styrene, isopropanol or terpinol.
A kind of 7. preparation process of Nano glass powder according to claim 1, it is characterised in that corase grinding zirconium ball
Sphere diameter in 3~20mm.
A kind of 8. preparation process of Nano glass powder according to claim 1, it is characterised in that fine grinding zirconium ball
Sphere diameter in 0.5~3mm.
A kind of 9. preparation process of Nano glass powder according to claim 1, it is characterised in that the Nano glass powder
The average grain diameter of Nano glass powder is in 60~120nm in suspension.
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| CN110600162A (en) * | 2019-10-23 | 2019-12-20 | 河南农业大学 | Solar cell conductive paste and preparation method thereof |
| CN110950540A (en) * | 2019-11-11 | 2020-04-03 | 上海银浆科技有限公司 | Surface modification method of glass for front silver paste of solar cell |
| CN112499977A (en) * | 2020-11-30 | 2021-03-16 | 华东理工大学 | Superfine silicate glass powder and preparation method thereof |
| CN113461338A (en) * | 2021-08-05 | 2021-10-01 | 江苏正能电子科技有限公司 | Nano glass powder for PERC back silver and preparation method thereof |
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| CN113617496B (en) * | 2021-08-06 | 2023-01-10 | Oppo广东移动通信有限公司 | Preparation method of nano glass powder, nano glass powder and glass product |
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