CN110590167A - Preparation method and application of hybrid glass powder - Google Patents
Preparation method and application of hybrid glass powder Download PDFInfo
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- CN110590167A CN110590167A CN201910942166.8A CN201910942166A CN110590167A CN 110590167 A CN110590167 A CN 110590167A CN 201910942166 A CN201910942166 A CN 201910942166A CN 110590167 A CN110590167 A CN 110590167A
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- glass powder
- graphene
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- 239000011521 glass Substances 0.000 title claims abstract description 69
- 239000000843 powder Substances 0.000 title claims abstract description 68
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 48
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 39
- 229910052709 silver Inorganic materials 0.000 claims abstract description 20
- 239000004332 silver Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 14
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 30
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 15
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- 230000009471 action Effects 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 9
- 238000002604 ultrasonography Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000003638 chemical reducing agent Substances 0.000 claims description 7
- 229960005070 ascorbic acid Drugs 0.000 claims description 6
- 235000010323 ascorbic acid Nutrition 0.000 claims description 6
- 239000011668 ascorbic acid Substances 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000012046 mixed solvent Substances 0.000 claims description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 abstract description 11
- 230000008569 process Effects 0.000 abstract description 8
- 230000000052 comparative effect Effects 0.000 description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 229910052710 silicon Inorganic materials 0.000 description 3
- 239000010703 silicon Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 description 1
- 238000012935 Averaging Methods 0.000 description 1
- 229910003069 TeO2 Inorganic materials 0.000 description 1
- XNRNVYYTHRPBDD-UHFFFAOYSA-N [Si][Ag] Chemical compound [Si][Ag] XNRNVYYTHRPBDD-UHFFFAOYSA-N 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 229910021419 crystalline silicon Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000012776 electronic material Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 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
- 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
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/36—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal
- C03C17/3602—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer
- C03C17/3644—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating being a metal the metal being present as a layer the metal being silver
-
- 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
- H01B1/16—Conductive material dispersed in non-conductive inorganic material the conductive material comprising metals or alloys
-
- 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
Abstract
The application discloses preparation method and application of hybrid glass powder, the graphene is coated on the glass powder at first, then silver is deposited, the glass powder coated with the graphene and the silver is obtained, in the high-temperature sintering process, the graphene can form good ohmic contact on an interface, and meanwhile, a silver layer coated on the surface of the graphene can improve the wettability of silver powder, reduce the generation of interface holes in the sintering process of the silver powder, and improve the electrical property of a solar cell piece.
Description
Technical Field
The application relates to the technical field of electronic materials, in particular to a preparation method and application of hybrid glass powder.
Background
The conductive silver paste is a key material of the crystalline silicon solar cell, and directly influences the performance of the cell. The conductive silver paste mainly consists of 3 parts: conductive silver powder, glass powder and an organic phase. The silver powder is a conductive phase, the glass powder plays a role in binding, promoting the silver powder to be melted and forming a medium substance of silver-silicon ohmic contact in the sintering process, and the organic phase plays a role in dispersing and endowing the slurry with fluidity.
The glass powder only accounts for a small proportion in the silver paste, but is an important factor influencing the sintering effect of the silver powder, the corrosion degree of the silicon surface, the contact resistance and other properties, and particularly whether good ohmic contact can be formed with the silicon after sintering is a key for improving the photoelectric conversion efficiency of the solar cell. Therefore, in the prior art, a certain amount of oxide is mostly added into the glass powder to improve the wetting capacity of silver in the sintering process, so as to obtain a more compact electrode structure. However, the glass powder has different expansion coefficients of all components, and the silver powder also shrinks in the sintering process, so that pores are easy to generate on an Ag/Si interface, and the improvement of the battery performance is limited.
Graphene has excellent electrical properties, the resistance of the graphene is lower than that of silver, and part of the technology uses graphene to replace part of silver powder so as to obtain lower parallel resistance. However, this method mainly considers the improvement of the conductive phase performance, and has a limited effect on the improvement of the interface contact resistance.
Disclosure of Invention
The specific embodiment of the application provides a preparation method and application of hybrid glass powder, wherein graphene and silver are attached to the surface of the glass powder, so that interface contact resistance is reduced, and wettability of silver powder is improved. The adopted technical scheme is as follows:
in one aspect, a method for preparing a hybrid glass frit is provided, comprising:
dispersing graphene in water to prepare graphene suspension;
preparing a mixed solvent of water and isopropanol, adding glass powder for uniform dispersion, sequentially adding a silane coupling agent and the graphene suspension prepared in the previous step, performing ultrasonic dispersion and heating, and washing and drying to prepare graphene-coated glass powder;
adding the prepared graphene-coated glass powder into a silver nitrate solution under the action of ultrasound and stirring, uniformly dispersing, maintaining the action of ultrasound stirring unchanged, adding a reducing agent to deposit silver on the surface of the powder, washing and drying to obtain the hybrid glass powder.
Preferably, the reducing agent is ascorbic acid.
Preferably, the weight ratio of the glass powder to the graphene to the silver nitrate is 1: 0.005-0.05: 0.5-1.
Preferably, the sheet diameter of the graphene is 0.1-0.5 μm, and the particle diameter of the glass powder is 1-4 μm.
Preferably, the concentration of the silver nitrate solution is 0.5-2 mol/L.
Preferably, the amount of the silane coupling agent is 0.5-5% of the weight of the glass powder.
In another aspect, a conductive silver paste is provided, which contains the hybrid glass powder prepared by the above method.
The technical scheme provided by the specific embodiment of the application has at least the following beneficial effects:
graphene has excellent electrical properties, the graphene is coated on glass powder at first, then silver is deposited to obtain the glass powder coated with graphene and silver, in the high-temperature sintering process, the graphene can form good ohmic contact at an interface, and meanwhile, a silver layer coated on the surface of the graphene can improve the wettability of silver powder, reduce the generation of interface holes in the silver powder sintering process and improve the electrical properties of a solar cell piece.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the following detailed description is further provided in conjunction with specific embodiments. The embodiments described herein are only some of the embodiments of the present application and should not be construed as limiting the scope of the present application.
The preparation method of the hybrid glass powder provided by the specific embodiment of the application comprises the following steps:
step 1, dispersing graphene in water to prepare graphene suspension. Preparing a mixed solvent of water and isopropanol, adding glass powder for uniform dispersion, sequentially adding a silane coupling agent and the prepared graphene suspension, ultrasonically dispersing, heating, washing and drying to obtain the graphene-coated glass powder.
At present, the glass powder mainly comprises lead-containing glass powder, and the components contain a certain amount of PbO. In order to reduce the harm and meet the requirement of environmental protection, the lead-free glass powder is preferably selected, and the optional raw materials comprise SiO2、Bi2O3、B2O3、SnO2、Fe2O3、TeO2、ZnO、Al2O3、TiO2And the particle size is preferably 1 to 4 μm. The graphene sheet diameter is preferably 0.1-0.5 mu m, the silane coupling agent is used for enabling the graphene sheet layer to be coated on the surface of the glass powder better, the amount of the silane coupling agent is preferably 0.5-5% of the weight of the glass powder, and in an exemplary embodiment, KH550 is adopted and is used in the amount of the glass powder3％。
And 2, adding the graphene-coated glass powder prepared in the step 1 into a silver nitrate solution under the action of ultrasound and stirring, uniformly mixing, adding a reducing agent under the condition to deposit silver on the surface of the powder, and washing and drying to prepare the hybrid glass powder after silver deposition is finished. The concentration of the silver nitrate solution can be 0.5-2 mol/L, and in order to obtain hybrid glass powder with good performance, the optimal weight ratio of the glass powder to the graphene to the silver nitrate is 1: 0.005-0.05: 0.5-1. The reducing agent may be ascorbic acid, hydrazine hydrate, etc., and is preferably ascorbic acid, and the reducing agent may be in excess.
According to the method, the glass powder is coated with the graphene, the coupling agent with the dispersion effect volatilizes in the high-temperature sintering process, the graphene dispersed on the interface can form good ohmic contact, meanwhile, the silver coated on the surface of the graphene can improve the wettability of the graphene on silver powder, so that the silver powder is better attached to the interface, the generation of interface holes is reduced, and the electrical property of the solar cell piece is improved.
Example 1
A method of making a hybrid glass frit comprising:
dispersing graphene in water to prepare graphene suspension;
preparing a mixed solvent (volume ratio is 1:9) of water and isopropanol, adding glass powder (lead-free glass powder with the particle size of 1-4 mu m) to be uniformly dispersed, then adding silane coupling agent KH550 with the amount of 3% of the weight of the glass powder, then adding the graphene suspension prepared in the previous step, performing ultrasonic dispersion, heating to 60-70 ℃, maintaining for 60min, filtering, washing and drying to obtain graphene-coated glass powder;
adding the prepared graphene-coated glass powder into 1mol/L silver nitrate solution under the action of ultrasound and stirring, uniformly dispersing, maintaining the action of ultrasound stirring, adding ascorbic acid to deposit silver on the surface of the powder, washing and drying to obtain the hybrid glass powder.
Wherein the weight ratio of the glass powder to the graphene to the silver nitrate is 1:0.05: 1.
Example 2
Compared with the example 1, the difference is that the concentration of the silver nitrate solution is 0.5mol/L, and the weight ratio of the glass powder, the graphene and the silver nitrate is 1:0.01: 0.5.
Comparative example 1
Adding glass powder (same type as example 1) into 1mol/L silver nitrate solution under the action of ultrasound and stirring, wherein the weight ratio of the glass powder to the silver nitrate is 1:1, uniformly dispersing, maintaining the action of ultrasound stirring, adding ascorbic acid to deposit silver on the surface of the glass powder, washing and drying to obtain the hybrid glass powder.
The glass powder prepared in each example and each comparative example is prepared into the front silver paste of the solar cell according to the following weight ratio: 90 parts of silver powder with the particle size of 1-3 mu m, 10 parts of nano silver powder with the particle size of 50-100 nm, 10 parts of organic carrier, 5 parts of hybrid glass powder and 1 part of graphene. The preparation method of the slurry comprises the following steps: the components are mixed evenly and ground to the fineness of less than 10 mu m.
Printing the prepared front silver paste on a 156 mm-156 mm silicon chip with the thickness of 180-190 mu, drying, sintering and cooling to obtain a solar cell, testing electrical performance parameters, testing twice, and averaging to obtain the result shown in table 1, wherein Uoc is open-circuit voltage, Isc is short-circuit current, and Eff is conversion efficiency. It can be seen that the electrical performance parameters of the batteries of examples 1 and 2 are higher than those of comparative example 1 by using the hybrid glass powder coated with graphene and silver.
TABLE 1
| Glass frit type | Uoc(V) | Isc(A) | Eff(％) |
| Example 1 | 0.6305 | 8.9901 | 18.5137 |
| Example 2 | 0.6300 | 8.9035 | 18.4259 |
| Comparative example 1 | 0.6297 | 8.8783 | 18.2516 |
Claims (7)
1. A method for preparing hybrid glass powder is characterized by comprising the following steps:
dispersing graphene in water to prepare graphene suspension;
preparing a mixed solvent of water and isopropanol, adding glass powder for uniform dispersion, sequentially adding a silane coupling agent and the graphene suspension prepared in the previous step, performing ultrasonic dispersion and heating, and washing and drying to prepare graphene-coated glass powder;
adding the prepared graphene-coated glass powder into a silver nitrate solution under the action of ultrasound and stirring, uniformly dispersing, maintaining the action of ultrasound stirring unchanged, adding a reducing agent to deposit silver on the surface of the powder, washing and drying to obtain the hybrid glass powder.
2. The method for preparing hybrid glass frit according to claim 1, wherein the reducing agent is ascorbic acid.
3. The preparation method of hybrid glass powder according to claim 1, wherein the weight ratio of the glass powder to the graphene to the silver nitrate is 1: 0.005-0.05: 0.5-1.
4. The preparation method of hybrid glass powder according to claim 1 or 3, wherein the graphene has a sheet diameter of 0.1-0.5 μm, and the glass powder has a particle diameter of 1-4 μm.
5. The preparation method of hybrid glass powder according to claim 1 or 3, wherein the concentration of the silver nitrate solution is 0.5-2 mol/L.
6. The preparation method of hybrid glass powder according to claim 1, wherein the amount of the silane coupling agent is 0.5-5% by weight of the glass powder.
7. Conductive silver paste, characterized in that it contains hybrid glass frit obtained by the preparation method according to any one of claims 1 to 6.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910942166.8A CN110590167B (en) | 2019-09-30 | 2019-09-30 | Preparation method and application of hybrid glass powder |
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| CN201910942166.8A CN110590167B (en) | 2019-09-30 | 2019-09-30 | Preparation method and application of hybrid glass powder |
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| CN110590167B CN110590167B (en) | 2022-06-21 |
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Cited By (2)
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| CN113698104A (en) * | 2021-10-19 | 2021-11-26 | 西北大学 | Bismuth trioxide nano-layer modified lead-free glass powder and preparation method thereof |
| CN114456757A (en) * | 2022-01-27 | 2022-05-10 | 湖南创瑾技术研究院有限公司 | Pouring sealant and preparation method and application thereof |
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| Publication number | Publication date |
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| CN110590167B (en) | 2022-06-21 |
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