CN109422461A - Microbead glass and its preparation process for conductive silver paste - Google Patents
Microbead glass and its preparation process for conductive silver paste Download PDFInfo
- Publication number
- CN109422461A CN109422461A CN201710778694.5A CN201710778694A CN109422461A CN 109422461 A CN109422461 A CN 109422461A CN 201710778694 A CN201710778694 A CN 201710778694A CN 109422461 A CN109422461 A CN 109422461A
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- Prior art keywords
- glass
- parts
- microbead
- oxide
- pearl
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- 239000011521 glass Substances 0.000 title claims abstract description 91
- 239000011325 microbead Substances 0.000 title claims abstract description 37
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 22
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims abstract description 15
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims abstract description 15
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000005642 Oleic acid Substances 0.000 claims abstract description 15
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims abstract description 15
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims abstract description 15
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims abstract description 15
- RBNWAMSGVWEHFP-UHFFFAOYSA-N trans-p-Menthane-1,8-diol Chemical compound CC(C)(O)C1CCC(C)(O)CC1 RBNWAMSGVWEHFP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000004005 microsphere Substances 0.000 claims abstract description 13
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000011247 coating layer Substances 0.000 claims abstract description 11
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 11
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 11
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 11
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004327 boric acid Substances 0.000 claims abstract description 9
- 229910001947 lithium oxide Inorganic materials 0.000 claims abstract description 9
- 229910000476 molybdenum oxide Inorganic materials 0.000 claims abstract description 9
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 claims abstract description 9
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 claims abstract description 9
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910001930 tungsten oxide Inorganic materials 0.000 claims abstract description 9
- 239000011787 zinc oxide Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 229910000416 bismuth oxide Inorganic materials 0.000 claims abstract description 7
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims description 28
- 238000007667 floating Methods 0.000 claims description 11
- 238000000498 ball milling Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011324 bead Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 229910000831 Steel Inorganic materials 0.000 claims description 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 3
- 239000012634 fragment Substances 0.000 claims description 3
- 150000002576 ketones Chemical class 0.000 claims description 3
- 239000005416 organic matter Substances 0.000 claims description 3
- 229920006316 polyvinylpyrrolidine Polymers 0.000 claims description 3
- 238000010791 quenching Methods 0.000 claims description 3
- 230000000171 quenching effect Effects 0.000 claims description 3
- 239000010959 steel Substances 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims 1
- 239000002002 slurry Substances 0.000 abstract description 19
- 238000007639 printing Methods 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 9
- 238000005245 sintering Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000013461 design Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 229910052797 bismuth Inorganic materials 0.000 description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-UHFFFAOYSA-N 0.000 description 1
- FPZWZCWUIYYYBU-UHFFFAOYSA-N 2-(2-ethoxyethoxy)ethyl acetate Chemical compound CCOCCOCCOC(C)=O FPZWZCWUIYYYBU-UHFFFAOYSA-N 0.000 description 1
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 description 1
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical group CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- 230000010307 cell transformation Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000013082 photovoltaic technology Methods 0.000 description 1
- 239000011297 pine tar Substances 0.000 description 1
- 229940068124 pine tar Drugs 0.000 description 1
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
Classifications
-
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
-
- 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
- C03C12/00—Powdered glass; Bead compositions
-
- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
-
- 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
-
- 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
- H01B1/14—Conductive material dispersed in non-conductive inorganic material
-
- 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
-
- 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
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
-
- 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
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
- C03C2218/11—Deposition methods from solutions or suspensions
- C03C2218/111—Deposition methods from solutions or suspensions by dipping, immersion
Abstract
The present invention discloses a kind of microbead glass and its preparation process for conductive silver paste, and the microbead glass is grouped as by the group of following parts by weight: 10 ~ 50 parts of tellurium dioxide, 15 ~ 70 parts of bismuth oxide, 2 ~ 10 parts of zinc oxide, 1 ~ 15 part of tungsten oxide, 5 ~ 20 parts of lithia, 0.3 ~ 5 part of molybdenum oxide, 0.2 ~ 5 part of aluminium oxide, 0.3 ~ 5 part of boric acid, 0.2 ~ 2 part of silica；The partial size D50 of the glass microsphere powder is 1 ~ 2 μm；In the mixed liquor that the glass microsphere powder investment terpinol, butyl carbitol acetate, oleic acid and polyvinylpyrrolidone are formed, under 80 degree of heat-retaining conditions, stirs 3-6 hours, obtain the globular glass pearl with organic coating layer.Microbead glass of the present invention improves slurry system lubricity, increases strike through, avoids lacking material problem in thin grid line item, and slurry melten glass in sintering is not easy to flow, and keeps fine line style, is suitble to the printing of narrow opening halftone filament.
Description
Technical field
The present invention relates to a kind of microbead glass for conductive silver paste, belong to solar battery technical field of function materials.
Background technique
Photovoltaic cell has been achieved with development of advancing by leaps and bounds, photovoltaic cell as new cleaning fuel important branch in recent years
Technology be also it is with rapid changepl. never-ending changes and improvements, full industrial chain all actively by technological innovation promotion photovoltaic cell transformation efficiency and is reducing cost,
Cheap internet access is striven for, traditional high pollution energy is substituted.
Crystal silicon photovoltaic battery is the main type of current photovoltaic cell, 90% or more accounting, photoelectricity transformation principle are as follows: boron
The P-type silicon of doping and the N-type silicon of phosphorus doping form PN junction, and when sunlight irradiation, PN junction is absorbed by photon energy excitation electricity
Sub- transition forms electron-hole pair, to generate electric current.According to law of conservation of energy, absorption photon energy is more, photovoltaic electric
Pond transformation efficiency is higher.Crystal silicon photovoltaic technology generallys use light-receiving surface coated with antireflection film layer at present, in addition, reducing light-receiving surface electricity
Pole grid line blocks two aspects to increase absorbing amount.
Crystal silicon solar batteries light-receiving surface electrode is generally by screen printing mode by conducting paste (silver paste) by preparatory
Design configuration is printed to be formed, and re-sinters to be formed, and is generally divided into main grid and thin grid two parts.Fine lines printing as described below refers to
Thin gate part.Reducing grid line and blocking light source is mainly to pass through the depth-width ratio for improving the thin grid of battery light-receiving surface, in battery design technology
The current the main direction of development of aspect is the close grid design of the thin grid of high square resistance, such as publication CN201420731827.5 and
Described in CN201210196890.9；In terms of printing technology, just like metal foil described in publication CN201220204596.3
Halftone technology, the screen template technology as described in publication CN201210047834.9 and CN201520597633.5 are such as public
Open secondary printing halftone technology etc. described in patent CN201520495081.7.In order to reach fine lines purpose, screen mesh printing plate is thin
Grid opening design is more and more narrow, shows according to open source information, several years ago with 20-30 μm/year decrease of speed, in recent years since slurry prints
The limitation of brush performance, the annual thin grid opening of halftone reduce 3-5 μm or so.Screen mesh printing plate is open narrow slurry printing strike through with regard to poor,
It is easy to cause thin grid after printing locally to lack material situation, to increase cell series resistance, influences solar cell photoelectric conversion effect
Rate.
Summary of the invention
The present invention provides a kind of microbead glass for conductive silver paste, which has high temperature
Viscosity is big, the big feature of surface tension, improves slurry system lubricity, increases strike through, avoids lacking material problem in thin grid line item,
Slurry melten glass in sintering is not easy to flow, and keeps fine line style, narrow opening halftone filament is suitble to print, intact material situation,
Line width, depth-width ratio is big, short circuit current and high conversion efficiency；Meanwhile providing a kind of system of microbead glass for conductive silver paste
Standby technique.
In order to achieve the above objectives, the microbead glass technical solution that the present invention uses is: a kind of microballon for conductive silver paste
Glass, the microbead glass are grouped as by the group of following parts by weight:
10 ~ 50 parts of tellurium dioxide,
15 ~ 70 parts of bismuth oxide,
2 ~ 10 parts of zinc oxide,
1 ~ 15 part of tungsten oxide,
5 ~ 20 parts of lithia,
0.3 ~ 5 part of molybdenum oxide,
0.2 ~ 5 part of aluminium oxide,
0.3 ~ 5 part of boric acid,
0.2 ~ 2 part of silica；
The partial size D50 of the glass microsphere powder is 0.5 ~ 4 μm；
The mixing that the glass microsphere powder investment terpinol, butyl carbitol acetate, oleic acid and polyvinylpyrrolidone are formed
In liquid, under 60-90 degree heat-retaining condition, stirs 3-6 hours, obtain the globular glass pearl with organic coating layer.
Further improved technical solution in above-mentioned technical proposal is as follows:
In above scheme, the terpinol, butyl carbitol acetate, oleic acid and polyvinylpyrrolidone are according to 100:(80-
120): (15-35): (15-35) weight ratio is mixed to form mixed liquor.
In order to achieve the above objectives, the microbead glass and its fabricating technology scheme that the present invention uses are: being used for conductive silver
The microbead glass and its preparation process of slurry, comprising the following steps:
Step 1: by 10 ~ 50 parts of tellurium dioxide, 15 ~ 70 parts of bismuth oxide, 2 ~ 10 parts of zinc oxide, 1 ~ 15 part of tungsten oxide, lithia 5 ~
20 parts, 0.3 ~ 5 part of molybdenum oxide, 0.2 ~ 5 part of aluminium oxide, 0.3 ~ 5 part of boric acid, 0.2 ~ 2 part of silica melted at 700 ~ 1000 degree, protect
Temperature；
Step 2: molten liquid is carried out water quenching cooling, steel plate cooling or the cooling of the twin rollers type of cooling, soaking time is 0.5 ~ 2
Hour；
Step 3: obtaining glass powder, ball milling by planetary ball mill ball milling after glass fragment is ground；
Step 4: glass powder is uniformly put by distributing device by flame floating method Cheng Zhu in beading stove, in glass
Globular glass pearl is formed under surface tension effects, when particle is heated into pearl and is in floating state, after cooling system is cooling
Into collector, the preferable solid glass micro-bead of sphericity is obtained, the stick to each other between bead is prevented, is heated into pearl in particle
While be in floating state, collector is being entered after cooling system is cooling, is obtaining the preferable solid glass micro-bead of sphericity；
Step 5: the globular glass pearl powder is put into terpinol, butyl carbitol acetate, oleic acid and polyvinylpyrrolidine
It in the mixed liquor that ketone is formed, keeps the temperature and stirs, form the globular glass pearl with organic coating layer；
Step 6: the globular glass pearl with organic coating layer obtained with dehydrated alcohol washing step five, by remaining organic matter
Washes clean, and dry acquisition microbead glass in an oven.
Further improved technical solution in above-mentioned technical proposal is as follows:
1. in above scheme, the soaking time of the step 2 is 0.5 ~ 2 hour.
2. in above scheme, the Ball-milling Time of the step 3 is 1 ~ 3 hour.
3. in above scheme, the condition of the step 4 is the heating melting in the hot high temperature gas flow of 0.5MPa.
4. in above scheme, the temperature of the step 5 heat preservation is 80 degree, and mixing time is 3 ~ 6 hours.
5. in above scheme, oven temperature is 100 degree lower 1 hour dry in the step 6.
Since above-mentioned technical proposal is used, the present invention has following advantages and effect compared with prior art:
1. the present invention is used for the microbead glass and its preparation process of conductive silver paste, use by 10 ~ 50 parts of tellurium dioxide, oxidation
15 ~ 70 parts of bismuth, 2 ~ 10 parts of zinc oxide, 1 ~ 15 part of tungsten oxide, 5 ~ 20 parts of lithia, 0.3 ~ 5 part of molybdenum oxide, 0.2 ~ 5 part of aluminium oxide,
0.3 ~ 5 part of boric acid, 0.2 ~ 2 part of the silica glass microsphere powder formed, glass microballoon big, big spy of surface tension with high temperature viscosity
Point, slurry melten glass in sintering are not easy to flow, and keep fine line style；Slurry system lubricity is improved, strike through is increased,
It avoids lacking material problem in thin grid line item, slurry melten glass in sintering is not easy to flow, and is suitble to the printing of narrow opening halftone filament, nothing
Material situation is lacked, line width, depth-width ratio is big, short circuit current and high conversion efficiency；Secondly, its glass microsphere powder puts into terpinol, fourth
In the mixed liquor that base carbitol acetate, oleic acid and polyvinylpyrrolidone are formed, under 80 degree of heat-retaining conditions, stir 3-6 hours,
The globular glass pearl with organic coating layer is obtained, glass microballoon in the slurry uniformly dispersed is improved, avoids reuniting, is increased
Stability of Slurry and printing continuity, improve printing stability.
2. the present invention is used for the microbead glass and its preparation process of conductive silver paste, pearl is heated into particle and is in floating
When state, collector is being entered after cooling system is cooling, is obtaining the preferable solid glass micro-bead of sphericity, prevented between bead
Stick to each other, floating state is in while particle is heated into pearl, collector is being entered after cooling system is cooling, is being obtained
The preferable solid glass micro-bead of sphericity.
Specific embodiment
The present invention will be further described below with reference to examples:
Embodiment 1 ~ 4: a kind of microbead glass for conductive silver paste, the microbead glass are grouped as by the group of following parts by weight,
The glass microsphere powder is composed of the following components:
Table 2
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | |
| Tellurium dioxide | 12 parts | 30 parts | 45 parts | 24 parts |
| Bismuth oxide | 45 parts | 30 parts | 60 parts | 28 parts |
| Zinc oxide | 8 parts | 3 parts | 5 parts | 6 parts |
| Tungsten oxide | 4 parts | 12 parts | 6 parts | 10 parts |
| Lithia | 9 parts | 16 parts | 6 parts | 18 parts |
| Molybdenum oxide | 1.6 part | 0.6 part | 2 parts | 3.2 part |
| Aluminium oxide | 2 parts | 0.5 part | 3 parts | 4 parts |
| Boric acid | 1.8 part | 3 parts | 2 parts | 1 part |
| Silica | 1.2 part | 0.8 part | 1.6 part | 1.4 part |
The partial size D50 of the glass microsphere powder is 0.5 ~ 4 μm；
The mixing that the glass microsphere powder investment terpinol, butyl carbitol acetate, oleic acid and polyvinylpyrrolidone are formed
In liquid, under 80 degree of heat-retaining conditions, stirs 3 ~ 6 hours, obtain the globular glass pearl with organic coating layer
Terpinol, butyl carbitol acetate, oleic acid and polyvinylpyrrolidone are according to 100:85:25:32 weight in embodiment 1
Than being mixed to form mixed liquor；In embodiment 2 terpinol, butyl carbitol acetate, oleic acid and polyvinylpyrrolidone according to
100:100:18:20 weight ratio is mixed to form mixed liquor；Terpinol, butyl carbitol acetate, oleic acid and poly- second in embodiment 3
Alkene pyrrolidone is mixed to form mixed liquor according to 100:110:30:30 weight ratio；Terpinol, butyl carbitol vinegar in embodiment 4
Acid esters, oleic acid and polyvinylpyrrolidone are mixed to form mixed liquor according to 100:90:20:18 weight ratio.
A kind of preparation process for above-mentioned microbead glass, comprising the following steps:
Step 1: by 10 ~ 50 parts of tellurium dioxide, 15 ~ 70 parts of bismuth oxide, 2 ~ 10 parts of zinc oxide, 1 ~ 15 part of tungsten oxide, lithia 5 ~
20 parts, 0.3 ~ 5 part of molybdenum oxide, 0.2 ~ 5 part of aluminium oxide, 0.3 ~ 5 part of boric acid, 0.2 ~ 2 part of silica melted at 700 ~ 1000 degree, protect
Temperature；
Step 2: molten liquid is carried out water quenching cooling, steel plate cooling or the cooling of the twin rollers type of cooling, soaking time is 0.5 ~ 2
Hour；
Step 3: obtaining glass powder by planetary ball mill ball milling after glass fragment is ground, Ball-milling Time is 1 ~ 3 small
When；
Step 4: glass powder is uniformly put by distributing device by flame floating method Cheng Zhu in beading stove, in glass
Globular glass pearl is formed under surface tension effects, condition is the heating melting in the hot high temperature gas flow of 0.5MPa；
Step 5: the globular glass pearl powder is put into terpinol, butyl carbitol acetate, oleic acid and polyvinylpyrrolidine
In the mixed liquor that ketone is formed, under 80 degree of heat-retaining conditions, stirs 3-6 hours, form the globular glass pearl with organic coating layer；
Organic coating frit is obtained for several times Step 6: being washed in the 6th step with dehydrated alcohol, by remaining organic matter washes clean,
And in an oven 100 degree it is 1 hour lower dry, arrive evenly dispersed glass microballoon.
Four condition of above-mentioned steps is the heating melting in the hot high temperature gas flow of 0.5MPa.
Between above-mentioned steps four and step 5 when particle is heated into pearl and is in floating state, after cooling system is cooling
Into collector, the preferable solid glass micro-bead of sphericity is obtained, the stick to each other between bead is prevented, is heated into pearl in particle
While be in floating state, collector is being entered after cooling system is cooling, is obtaining the preferable solid glass micro-bead of sphericity.
The glass microballoon that embodiment 1 ~ 4 is obtained with organic carrier and dispersant, is ground according to a certain ratio through three rollers
After add silver powder mixing, slurry is made after three rollers.
Slurry with 1 ~ 4 glass microballoon of embodiment, test result are as shown in table 3:
Table 3
When using above-mentioned microbead glass and its preparation process for conductive silver paste, use by 10 ~ 50 parts of tellurium dioxide, oxygen
Change 15 ~ 70 parts of bismuth, 2 ~ 10 parts of zinc oxide, 1 ~ 15 part of tungsten oxide, 5 ~ 20 parts of lithia, 0.3 ~ 5 part of molybdenum oxide, aluminium oxide 0.2 ~ 5
Part, 0.3 ~ 5 part of boric acid, 0.2 ~ 2 part of the silica glass microsphere powder formed, glass microballoon big, surface tension with high temperature viscosity
Big feature, slurry melten glass in sintering are not easy to flow, and keep fine line style；Slurry system lubricity is improved, is increased saturating
Mo Xing avoids lacking material problem in thin grid line item, and slurry melten glass in sintering is not easy to flow, and is suitble to narrow opening halftone filament print
Brush, intact material situation, line width, depth-width ratio is big, short circuit current and high conversion efficiency；Secondly, its glass microsphere powder puts into pine tar
In the mixed liquor that alcohol, butyl carbitol acetate, oleic acid and polyvinylpyrrolidone are formed, under 80 degree of heat-retaining conditions, 3-6 is stirred
Hour, the globular glass pearl with organic coating layer is obtained, uniformly dispersed, the group of avoiding of glass microballoon in the slurry is improved
It is poly-, increase Stability of Slurry and printing continuity, improves printing stability.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
Scholar cans understand the content of the present invention and implement it accordingly, and it is not intended to limit the scope of the present invention.It is all according to the present invention
Equivalent change or modification made by Spirit Essence, should be covered by the protection scope of the present invention.
Claims (8)
1. a kind of microbead glass for conductive silver paste, it is characterised in that: the microbead glass is grouped by the group of following parts by weight
At:
10 ~ 50 parts of tellurium dioxide,
15 ~ 70 parts of bismuth oxide,
2 ~ 10 parts of zinc oxide,
1 ~ 15 part of tungsten oxide,
5 ~ 20 parts of lithia,
0.3 ~ 5 part of molybdenum oxide,
0.2 ~ 5 part of aluminium oxide,
0.3 ~ 5 part of boric acid,
0.2 ~ 2 part of silica；
The partial size D50 of the glass microsphere powder is 0.5 ~ 4 μm；
The mixing that the glass microsphere powder investment terpinol, butyl carbitol acetate, oleic acid and polyvinylpyrrolidone are formed
In liquid, under 60-90 degree heat-retaining condition, stirs 3-6 hours, obtain the globular glass pearl with organic coating layer.
2. the microbead glass according to claim 1 for conductive silver paste, it is characterised in that: the terpinol, butyl card
Must alcohol acetate, oleic acid and polyvinylpyrrolidone according to 100:(80-120): (15-35): (15-35) weight ratio is mixed to form
Mixed liquor.
3. a kind of preparation process for microbead glass described in claim 1, it is characterised in that: the following steps are included:
Step 1: by 10 ~ 50 parts of tellurium dioxide, 15 ~ 70 parts of bismuth oxide, 2 ~ 10 parts of zinc oxide, 1 ~ 15 part of tungsten oxide, lithia 5 ~
20 parts, 0.3 ~ 5 part of molybdenum oxide, 0.2 ~ 5 part of aluminium oxide, 0.3 ~ 5 part of boric acid, 0.2 ~ 2 part of silica melted at 700 ~ 1000 degree, protect
Temperature；
Step 2: molten liquid is carried out water quenching cooling, steel plate cooling or the cooling of the twin rollers type of cooling, soaking time is 0.5 ~ 2
Hour；
Step 3: obtaining glass powder, ball milling by planetary ball mill ball milling after glass fragment is ground；
Step 4: glass powder is uniformly put by distributing device by flame floating method Cheng Zhu in beading stove, in glass
Globular glass pearl is formed under surface tension effects, when particle is heated into pearl and is in floating state, after cooling system is cooling
Into collector, the preferable solid glass micro-bead of sphericity is obtained, the stick to each other between bead is prevented, is heated into pearl in particle
While be in floating state, collector is being entered after cooling system is cooling, is obtaining the preferable solid glass micro-bead of sphericity；
Step 5: the globular glass pearl powder is put into terpinol, butyl carbitol acetate, oleic acid and polyvinylpyrrolidine
It in the mixed liquor that ketone is formed, keeps the temperature and stirs, form the globular glass pearl with organic coating layer；
Step 6: the globular glass pearl with organic coating layer obtained with dehydrated alcohol washing step five, by remaining organic matter
Washes clean, and dry acquisition microbead glass in an oven.
4. the preparation process of microbead glass according to claim 1, it is characterised in that: the soaking time of the step 2 is
0.5 ~ 2 hour.
5. the preparation process of microbead glass according to claim 1, it is characterised in that: the Ball-milling Time of the step 3 is
1 ~ 3 hour.
6. the preparation process of microbead glass according to claim 1, it is characterised in that: the condition of the step 4 be
Heating melting in 0.5MPa hot high temperature gas flow.
7. the preparation process of microbead glass according to claim 1, it is characterised in that: oven temperature is in the step 6
100 degree lower 1 hour dry.
8. the preparation process of microbead glass according to claim 1, it is characterised in that: the temperature of step 5 heat preservation is
80 degree, mixing time is 3 ~ 6 hours.
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Application publication date: 20190305 |