CN101887764B - Method for preparing silicon-based solar front silver paste - Google Patents
Method for preparing silicon-based solar front silver paste Download PDFInfo
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- CN101887764B CN101887764B CN2010102110648A CN201010211064A CN101887764B CN 101887764 B CN101887764 B CN 101887764B CN 2010102110648 A CN2010102110648 A CN 2010102110648A CN 201010211064 A CN201010211064 A CN 201010211064A CN 101887764 B CN101887764 B CN 101887764B
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- 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
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- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
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Abstract
The invention discloses a method for preparing silicon-based solar front silver paste. The paste consists of 0.5 to 5 percent of glass powder, 40 to 85 percent of laminar silver powder, 5 to 45 percent of nano silver powder, 5 to 10 percent of organic carrier, 2 to 6 percent of solvent and 0.2 to 2 percent of auxiliary agent. The method mainly comprises the following steps of: (1) preparing the glass powder, (2) preparing the organic carrier, and (3) preparing the paste. According to the main design scheme of the invention, the printing height of a grid line and the conversion efficiency of a contact resistor and a battery can be changed by changing the adding proportion of the glass powder, the laminar silver powder and the nano silver powder; the viscosity and the printability of a product can be adjusted by changing the adding proportion of the organic carrier and the solvent; and the plasticity, leveling property and printability of the product can be adjusted by changing the adding proportion of a plasticizer. The paste of the invention has excellent printability, the sintered paste and a silicon chip form good alloy, a grid line electrode has great height, the series resistance is low, and the battery has high conversion efficiency.
Description
Technical field:
The invention belongs to technical field of electronic materials, relate to a kind of preparation method of silicon-based solar front silver paste.
Background technology:
Tradition fossil energy worsening shortages, the terrestrial climate variation issue long-term existence that causes because of excess discharging carbon dioxide isothermal chamber gas and growing in intensity, the more and more national people and government have realized that, the transformation of energy resource structure is imperative, being extensive use of of clean reproducible energies such as solar energy power generating become the tendency of the day, with moral, day is the advanced country of representative, owing to take the lead in having taked effective government subsidy policy, impel the demand of photovoltaic cell sharply to increase, also drive each photovoltaic of the world that comprises China and produced rapid emergence with market, China successively surmounts Germany, Japan began to become solar module producing country and exported country the biggest in the world in 2007.Meanwhile, also rousing oneself to catch up in the photovoltaic application market of countries such as the China and the U.S., Russia, India, South Africa, Eastern Europe, Southeast Asia, obtains considerable progress.
The technology of tool meaning during solar photovoltaic technology utilizes as solar energy, become countries in the world and competitively study the focus of application, nearest 10 years speed increases with every year average 30%, nearest 3 years especially with annual speed rapid growth more than 50%, industrialized development was the fastest after solar energy power generating had become renewable energy source domain relaying wind power generation, maximum industry, IC Insights prediction, the equipment investment of solar cell manufacturer will be stepped into development track in 2011, estimate to increase by 13% than the last year in 2011, reach 700,000,000 7,000 ten thousand dollars, 2012 year-on-years increase by 74%, reach 1,300,000,000 4,000 ten thousand dollars, to be extended to 1,900,000,000 7,000 ten thousand dollars (increasing by 47%) in 2013, surpass 1,400,000,000 7,000 ten thousand dollars of 08 year achievements than the last year.Estimate that factory's utilization of capacity also with steady-state growth, reached 63%, 2013 year and reaches 82% in 2011.
Summary of the invention:
The objective of the invention is to overcome network blocking and the dried net phenomenon that existing silver slurry is prone to when printing, and the low shortcoming of cell conversion efficiency behind the sintering, a kind of preparation method who is used for the silicon-based solar front silver paste of silk screen printing is provided.
A kind of preparation method who is used for the silicon-based solar front silver paste of silk screen printing, this slurry mainly is made up of glass dust 0.5～5%, flake silver powder 40～85%, nano-silver powder 5～45%, organic carrier 5%～10%, solvent 2%～6% and auxiliary agent 0.2%～2%.Network blocking and dried net phenomenon that main design of the present invention may occur when improving printing by proper auxiliary agent, organic carrier and solvent; By suitable glass system, flake silver powder, nano-silver powder, auxiliary agent improve behind the sintering that the gate line electrode height of silver powder and silicon chip is low, contact resistance and the low problem of cell conversion efficiency.
The objective of the invention is to solve by the following technical programs:
A kind of preparation method of silicon-based solar front silver paste, it comprises following basic step:
(1) preparation glass dust:
According to percentage by weight with 5%～30% SiO
2, 30%～75% PbO, 5%～30% B
2O
3, 2%～15% TiO
2And Al
2O
30.5%～10% mix, make the glass dust that average particle size range is 0.4 μ m～1.2 μ m through hot melt, cooling, pulverizing, ball milling, dried and screened; Described SiO
2, PbO, B
2O
3, TiO
2And Al
2O
3Total amount be 100%;
(2) preparation organic carrier:
According to percentage by weight, the ethyl cellulose resin with 10%～30% joins in 70%～90% the solvent, in Water Tank with Temp.-controlled dissolving fully, through 250～325 eye mesh screens filter organic carrier; The total amount of described ethyl cellulose resin and solvent is 100%;
(3) preparation slurry:
By weight percentage, glass dust with 0.5%～5%, 40～85% flake silver powder, 5～45% nano-silver powder, 5%～10% organic carrier, 2%～6% solvent and 0.2%～2% auxiliary agent mix in mixer, be dispersed on the three-roller below the 10 μ m again, after filter in 325～400 eye mesh screens and promptly get slurry; The total amount of described glass dust, flake silver powder, nano-silver powder, organic carrier, solvent and auxiliary agent is 100%.
Solvent described in the described step (2) adopts one or more mixed solution of butyl carbitol, butyl carbitol amyl acetate, terpinol.
The temperature of Water Tank with Temp.-controlled described in the described step (2) is 75 ℃～95 ℃.
Auxiliary agent comprises plasticizer and dispersant described in the described step (3), and plasticizer can be selected one or more of o-phthalic acid dibutyl ester, dibutyl phthalate (DBP), dioctyl adipate; Dispersant can be selected one or more of Tissuemat E, zinc stearate, microcrystalline wax.
Mixer described in the described step (3) is planetary or other type mixer.
The coefficient of expansion of glass dust is about 62 * 10 in the described step (1)
～7～75 * 10
～7/ K, sintering temperature are 500～650 ℃.
In the present invention, the adding proportion of change glass dust, flake silver powder and nano-silver powder can change the transformation efficiency of printing height, contact resistance and the battery of grid line; Viscosity, printing that the adding proportion of change organic carrier and solvent can be regulated product; Plasticity, levelability and printing that the adding proportion of change plasticizer can be regulated product.
Slurry of the present invention has excellent printing, the alloy that forms with silicon chip behind the sintering, and gate line electrode height height, series resistance is low, cell conversion efficiency is high.
Embodiment:
The invention discloses a kind of preparation method of silicon-based solar front silver paste, it comprises the steps:
(1) preparation glass dust:
A kind of glass system, it is formed and percentage by weight is respectively: 5%～30% SiO
2, 30%～75% PbO, 5%～30% B
2O
3, TiO
22%～15%, Al
2O
30.5%～10%.With above-mentioned glass system component mix, after hot melt, cooling, pulverizing, ball milling, drying, screen cloth sieve, making average particle size range is the glass dust of 0.4 μ m～1.2 μ m.
(2) preparation organic carrier:
With percentage by weight is that 10%～30% ethyl cellulose resin joins in 70%～90% the solvent, in Water Tank with Temp.-controlled dissolving fully, through 250～325 eye mesh screens filter organic carrier;
(3) preparation slurry:
0.5%～5% above-mentioned glass dust, 40～85% flake silver powder, 5～45% nano-silver powder, 5%～10% organic carrier, 2%～6% solvent and 0.2%～2% auxiliary agent mixed in mixer by weight percentage, be dispersed on the three-roller below the 10 μ m again, after filter in 325～400 eye mesh screens and promptly get slurry.
Vitreum described in the step (1) is Si-Pb～B glass system, and the coefficient of expansion is about (62～75) * 10
～7/ K, sintering temperature is at 500～650 ℃.
Each weight percentages of components sum of glass system described in the step (1) is 100%.
Solvent described in the step (2) adopts one or more mixed solutions of butyl carbitol, butyl carbitol amyl acetate, terpinol.
The temperature of Water Tank with Temp.-controlled described in the step (2) is 75 ℃～95 ℃.
Auxiliary agent comprises plasticizer and dispersant described in the step (3), and plasticizer can be selected one or more of o-phthalic acid dibutyl ester, dibutyl phthalate (DBP), dioctyl adipate; Dispersant can be selected one or more of Tissuemat E, zinc stearate, microcrystalline wax.
Mixer described in the step (3) is planetary or other type mixer.
Further specify preparation process of the present invention below in conjunction with concrete embodiment:
Embodiment 1
(1) preparation glass dust: percentage is with 5% SiO by weight
2, 75% PbO, 10% B
2O
3, 5% TiO
2, 5% Al
2O
3After mixing, after 900 ℃ insulation was melted in 30 minutes down, with the glass dust cold cut, ball milling 48 hours, standby through 400 eye mesh screens filtration back;
(2) preparation organic carrier: by weight percentage 10% ethyl cellulose resin is joined in 90% the butyl carbitol, in water bath with thermostatic control, is heated to 75 ℃～95 ℃ to dissolving fully, through 250 orders filter organic carrier;
(3) preparation slurry: by weight percentage with above-mentioned 0.5% glass dust, 40% flake silver powder, 45% nano-silver powder, 10% organic carrier, 3.5% butyl carbitol solvent, 0.6% dibutyl phthalate (DBP), 0.4% Tissuemat E dispersant, they are mixed in planetary or other mixer, be dispersed on the three-roller below the 10 μ m again, in 325 eye mesh screens, filter at last, record the front side silver paste that viscosity is 280kcps with Brookfield DV-II viscosimeter;
(4) use silk screen printing on 125*125 monocrystalline silicon piece (200 ± 20 μ m) in this slurry, drying, sintering, measuring the grid line height with the step instrument is 17.4 μ m; Test its electrical performance data with the monomer separator: series resistance 0.00987 Ω, transformation efficiency 17.8%.
Embodiment 2
(1) preparation glass dust: by weight percentage with 10% SiO
2, 65% PbO, 20% B
2O
3, 4% TiO
2, 1% Al
2O
3After mixing, after 950 ℃ insulation was melted in 30 minutes down, with the glass dust cold cut, ball milling 48 hours, standby through 400 eye mesh screens filtration back;
(2) preparation organic carrier: by weight percentage 15% ethyl cellulose resin is joined in 85% the butyl carbitol acetate, be heated to 75 ℃～95 ℃ to dissolving fully in water bath with thermostatic control, 325 orders filter;
(3) preparation slurry: by weight percentage with above-mentioned 1% glass dust, 85% flake silver powder, 5% nano-silver powder, 5% organic carrier, 3% butyl carbitol acetate solvent, 0.2% o-phthalic acid dibutyl ester, 0.8% zinc stearate dispersant, they are mixed in planetary or other mixer, be dispersed on the three-roller below the 10 μ m again, in 325 eye mesh screens, filter at last, record the front side silver paste that viscosity is 260kcps with Brookfield DV-II viscosimeter;
(4) use silk screen printing on 125*125 monocrystalline silicon piece (200 ± 20 μ m) in this slurry, drying, sintering, measuring the grid line height with the step instrument is 16.6 μ m; Test its electrical performance data with the monomer separator: series resistance 0.01023 Ω, transformation efficiency 17.4%.
Embodiment 3
(1) preparation glass dust: by weight percentage with 20% SiO
2, 70% PbO, 5% B
2O
3, 4.5% TiO
2, 0.5% Al
2O
3After mixing, after 930 ℃ insulation was melted in 30 minutes down, with the glass dust cold cut, ball milling 48 hours, standby through 325 eye mesh screens filtration back;
(2) preparation organic carrier: by weight percentage 20% ethyl cellulose resin is joined in 80% the terpinol, be heated to 75 ℃～95 ℃ to dissolving fully in water bath with thermostatic control, 325 orders filter;
(3) preparation slurry: by weight percentage with above-mentioned 3% glass dust, 60% flake silver powder, 25% nano-silver powder, 5% organic carrier, 6% terpinol solvent, 0.4% adipic acid dibutyl ester, 0.6% microcrystalline wax dispersant, they are mixed in planetary or other mixer, be dispersed on the three-roller below the 10 μ m again, in 400 eye mesh screens, filter at last, record the front side silver paste that viscosity is 290kcps with Brookfield DV-II viscosimeter;
(4) use silk screen printing on 125*125 monocrystalline silicon piece (200 ± 20 μ m) in this slurry, drying, sintering, measuring the grid line height with the step instrument is 15.8 μ m; Test its electrical performance data with the monomer separator: series resistance 0.01053 Ω, transformation efficiency 17.2%.
Embodiment 4
(1) preparation glass dust: by weight percentage with 30% SiO
2, 50% PbO, 10% B
2O
3, 5% TiO
2, 5% Al
2O
3After mixing, after 970 ℃ insulation was melted in 30 minutes down, with the glass dust cold cut, ball milling 48 hours, standby through 325 eye mesh screens filtration back;
(2) preparation organic carrier: by weight percentage 10% ethyl cellulose resin is joined in the terpinol of 40% butyl carbitol and 40%, be heated to 75 ℃～95 ℃ to dissolving fully in water bath with thermostatic control, 325 orders filter;
(3) preparation slurry: by weight percentage with above-mentioned 5% glass dust, 70% flake silver powder, 14% nano-silver powder, 8% organic carrier, 1% butyl carbitol and 1% terpinol solvent, 0.1% dibutyl phthalate (DBP) and 0.2% o-phthalic acid dibutyl ester, 0.3% Tissuemat E and 0.4% zinc stearate dispersant, they are mixed in planetary or other mixer, be dispersed on the three-roller below the 10 μ m again, in 400 eye mesh screens, filter at last, record the front side silver paste that viscosity is 275kcps with the BrookfieldDV-II viscosimeter;
(4) use silk screen printing on 125*125 monocrystalline silicon piece (200 ± 20 μ m) in this slurry, drying, sintering, measuring the grid line height with the step instrument is 15.4 μ m; Test its electrical performance data with the monomer separator: series resistance 0.01083 Ω, transformation efficiency 17.1%.
Embodiment 5
(1) preparation glass dust: by weight percentage with 20% SiO
2, 60% PbO, 13% B
2O
3, 2% TiO
2, 5% Al
2O
3After mixing, after 960 ℃ insulation was melted in 30 minutes down, with the glass dust cold cut, ball milling 48 hours, standby through 325 eye mesh screens filtration back;
(2) preparation organic carrier: by weight percentage 15% ethyl cellulose resin is joined in the terpinol of 20% butyl carbitol, 30% butyl carbitol amyl acetate and 35%, be heated to 75 ℃～95 ℃ to dissolving fully in water bath with thermostatic control, 325 orders filter;
(3) preparation slurry: by weight percentage with above-mentioned 2% glass dust, 70% flake silver powder, 15% nano-silver powder, 9% organic carrier, 1% butyl carbitol, 1% butyl carbitol amyl acetate and 0.5% terpinol solvent, 0.2% dibutyl phthalate (DBP), 0.2% o-phthalic acid dibutyl ester, 0.1% adipic acid dibutyl ester, 0.5% Tissuemat E dispersant, 0.3% zinc stearate, 0.2% microcrystalline wax, they are mixed in planetary or other mixer, be dispersed on the three-roller below the 10 μ m again, in 400 eye mesh screens, filter at last, record the front side silver paste that viscosity is 265kcps with Brookfield DV-II viscosimeter;
(4) use silk screen printing on 125*125 monocrystalline silicon piece (200 ± 20 μ m) in this slurry, drying, sintering, measuring the grid line height with the step instrument is 16.5 μ m; Test its electrical performance data with the monomer separator: series resistance 0.01013 Ω, transformation efficiency 17.5%.
Above content is to further describing that the present invention did in conjunction with concrete preferred implementation; can not assert that the specific embodiment of the present invention only limits to this; for the general technical staff of the technical field of the invention; without departing from the inventive concept of the premise; can also make some simple deduction or replace, all should be considered as belonging to the present invention and determine scope of patent protection by claims of being submitted to.
Claims (6)
1. the preparation method of a silicon-based solar front silver paste is characterized in that, it comprises following basic step:
(1) preparation glass dust:
According to percentage by weight with 5%～30% SiO
2, 30%～75% PbO, 5%～30% B
2O
3, 2%～15% TiO
2With 0.5%～10% Al
2O
3Mix, make the glass dust that average particle size range is 0.4 μ m～1.2 μ m through hot melt, cooling, pulverizing, ball milling, dried and screened; Described SiO
2, PbO, B
2O
3, TiO
2And Al
2O
3Total amount be 100%;
(2) preparation organic carrier:
According to percentage by weight, the ethyl cellulose resin with 10%～30% joins in 70%～90% the solvent, in Water Tank with Temp.-controlled dissolving fully, through 250～325 eye mesh screens filter organic carrier; The total amount of described ethyl cellulose resin and solvent is 100%;
(3) preparation slurry:
By weight percentage, glass dust with 0.5%～5%, 40～85% flake silver powder, 5～45% nano-silver powder, 5%～10% organic carrier, 2%～6% solvent and 0.2%～2% auxiliary agent mix in mixer, be dispersed on the three-roller below the 10 μ m again, after filter in 325～400 eye mesh screens and promptly get slurry; The total amount of described glass dust, flake silver powder, nano-silver powder, organic carrier, solvent and auxiliary agent is 100%.
2. according to the preparation method of the described a kind of silicon-based solar front silver paste of claim 1, it is characterized in that: solvent described in the described step (2) adopts one or more mixed solution of butyl carbitol, butyl carbitol amyl acetate, terpinol.
3. according to the preparation method of the described a kind of silicon-based solar front silver paste of claim 1, it is characterized in that: the temperature of Water Tank with Temp.-controlled described in the described step (2) is 75 ℃～95 ℃.
4. according to the preparation method of the described a kind of silicon-based solar front silver paste of claim 1, it is characterized in that: auxiliary agent comprises plasticizer and dispersant described in the described step (3), and plasticizer can be selected one or more of o-phthalic acid dibutyl ester, dibutyl phthalate (DBP), dioctyl adipate; Dispersant can be selected one or more of Tissuemat E, zinc stearate, microcrystalline wax.
5. according to the preparation method of the described a kind of silicon-based solar front silver paste of claim 1, it is characterized in that: mixer described in the described step (3) is planetary or other type mixer.
6. according to the preparation method of the described a kind of silicon-based solar front silver paste of claim 1, it is characterized in that: the coefficient of expansion of glass dust is about 62 * 10 in the described step (1)
～7～75 * 10
～7/ K, sintering temperature are 500～650 ℃.
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|---|---|---|---|
| CN2010102110648A CN101887764B (en) | 2010-06-28 | 2010-06-28 | Method for preparing silicon-based solar front silver paste |
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|---|---|---|---|
| CN2010102110648A CN101887764B (en) | 2010-06-28 | 2010-06-28 | Method for preparing silicon-based solar front silver paste |
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| CN101887764B true CN101887764B (en) | 2011-10-05 |
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| CN102903419B (en) * | 2012-09-27 | 2015-07-15 | 广州市儒兴科技开发有限公司 | Silver paste at front of crystalline silicon solar cell |
| CN103021567A (en) * | 2012-12-04 | 2013-04-03 | 彩虹集团公司 | Preparation method of front electrode silver paste for silicon-based solar energy |
| CN104347151A (en) * | 2013-08-02 | 2015-02-11 | 上海匡宇电子技术有限公司 | Conductive silver paste and preparation method thereof |
| CN103440897B (en) * | 2013-08-06 | 2017-03-01 | 浙江光达电子科技有限公司 | A kind of high square resistance silicon solar cell front silver electrode paste and preparation method thereof |
| EP2896602B1 (en) | 2014-01-16 | 2017-08-09 | Heraeus Precious Metals North America Conshohocken LLC | Low-silver electroconductive paste |
| CN106328246A (en) * | 2015-06-19 | 2017-01-11 | 江苏正能电子科技有限公司 | Positive silver paste for crystalline silicon solar cell |
| CN107731345B (en) * | 2016-07-05 | 2019-02-15 | 浙江光隆能源科技股份有限公司 | The preparation method of the back of solar cell silver paste of the anti-crack of the high-tensile strength of improvement |
| CN107234366A (en) * | 2017-06-16 | 2017-10-10 | 深圳市赛雅电子浆料有限公司 | One kind welds silver paste and its preparation technology and applies welding procedure |
| CN109897389A (en) * | 2017-12-07 | 2019-06-18 | 上海太阳能工程技术研究中心有限公司 | A kind of crystal silicon solar batteries front side silver paste organic carrier and preparation method |
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| US2945057A (en) * | 1959-04-01 | 1960-07-12 | Eastman Kodak Co | Preparation of methyl methacrylate |
| CN1045454C (en) * | 1996-03-12 | 1999-10-06 | 尹维平 | Inorganic electric-conductive coating and its preparation |
| CN1059287C (en) * | 1996-03-12 | 2000-12-06 | 尹维平 | Inorganic resistive coating and its preparation method |
| CN101609849B (en) * | 2009-07-13 | 2010-11-03 | 中南大学 | Silver conductive paste used for positive electrode of solar battery and preparation technique thereof |
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