CN103160211A - Solar crystalline silicon rod splicing glue and preparation method thereof - Google Patents
Solar crystalline silicon rod splicing glue and preparation method thereof Download PDFInfo
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- CN103160211A CN103160211A CN2011104271884A CN201110427188A CN103160211A CN 103160211 A CN103160211 A CN 103160211A CN 2011104271884 A CN2011104271884 A CN 2011104271884A CN 201110427188 A CN201110427188 A CN 201110427188A CN 103160211 A CN103160211 A CN 103160211A
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Abstract
The invention relates to solar crystalline silicon rod splicing glue and a preparation method thereof. The solar crystalline silicon rod splicing glue is composed of anaerobic liquid cement and accelerant. The preparation method comprises a step of respectively preparing the anaerobic liquid cement and the accelerant. When the solar crystalline silicon rod splicing glue is used, the accelerant is coated on the surface of a crystalline silicon rod to be sticked, then the crystalline silicon rod sticked with the accelerant is aired, the anaerobic liquid cement is coated on the accelerant of the crystalline silicon rod, and adhesion is fast carried out after the process of butt joint. According to the solar crystalline silicon rod splicing glue, under a premise that enough strength and toughness exist in the process of cutting crystal plates, the solar crystalline silicon rod splicing glue has the advantages of being fast in positioning time, convenient to operate and good in chemical-medium-resisting property and storage stability. The solar crystalline silicon rod splicing glue can become a first choice of adhesive for industries.
Description
Technical field
The present invention relates to a kind of sun power crystalline silicon rod splicing glue and preparation method thereof.
Background technology
In recent years, China's photovoltaic industry development is swift and violent, become the industry with stronger international competitiveness few in number in new industry, its basic reason is that Chinese photovoltaic enterprise adheres to technical research and cost control, to improve core competitiveness, the center of gravity of world's photovoltaic industry is shifted gradually to China.The technological process of production of photovoltaic industry solar cell is generally: ingot casting → butt → section → assembly → assembling.
At present, sun power crystalline silicon rod splicing glue generally adopts bi-component epoxide-resin glue.Epoxy resin glue has advantages of that bonding strength is high, but has simultaneously many significant shortcomings, and be embodied in: the silicon rod solidified and located time is long, and it is rapid that joint is produced in impact, even adopt quick curing agent also to be difficult to satisfy the rapid requirement of joint; Polyamines Curing Agents of Epoxy Resins is poisonous, and larger to the operating environment pollution, the operator often stimulates irritated grade for untoward reaction; The decay of bonding strength and modulus descends larger in water-based/oiliness cutting fluid environment; Troublesome poeration, the first and second component proportions are strict, and mixing must be evenly; Responsive to temperature and humidity, poor storage stability the surface skining denaturalization phenomenon easily occurs under permanent condition of storage, sheet even occurs falling when serious or fall excellent major accident.
Summary of the invention
Spell in order to solve in prior art epoxy resin used that sticklac existing setting time is long, intensity is low, the shortcomings such as poor impact toughness, troublesome poeration, ambient moisture sensitivity, poor storage stability, the invention provides a kind of sun power crystalline silicon rod splicing glue, it has the advantages such as easy to operate, that setting time is fast, bonding strength is high, toughness is good, resistant to chemical media is good, stability in storage is good, brings great improvement for spelling sticklac performance.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of sun power crystalline silicon rod splicing glue, formed by anaerobic gelatin and promotor,
Wherein, described anaerobic gelatin is comprised of each raw material of following parts by weight: 10～30 parts of thinners, and 20～80 parts of oligopolymers, 1～5 part of coupling agent, 1～5 part, oxygenant, 0.2～0.8 part of reductive agent helps 0.1～0.5 part of reductive agent, 0.01～0.03 part of stopper; Described surface promoter is comprised of each raw material of following parts by weight: 0.1～1 part of metal organic acid salt, 90～99.9 parts of solvents.
The invention has the beneficial effects as follows: the present invention is directed to sun power crystalline silicon rod splicing special adhesive technique and performance requriements, take the anaerobic glue compound monomer of special component as the main body composition, be equipped with again the auxiliary agents such as corresponding toughener, oxygenant, reductive agent, stopper, become the special-purpose anaerobic glue of silicon rod splicing.Again by add metal organic acid salt in the component of surface promoter, abandon the noxious solvents such as traditional acetone, chloroform, adopt nontoxic dehydrated alcohol to make solvent, shorten adhesive solidification thing setting time with this, improve stability in storage, bonding strength, impelling strength, improve technological operation and resistant to chemical media, reduce the moisture-sensitive degree of environment; And the performance comparison test of anaerobic adhesive of the present invention and traditional epoxy resin adhesive is estimated.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described thinner is one or more the mixing in the many acrylate of tetraethylene-glycol, hydroxyethyl methylacrylate, 2-phenoxyethyl acrylate.
Further, described oligopolymer is one or more the mixing in ethoxyquin bisphenol a dimethacrylate (the preferred commercially available Changxing BPA2EODMA of chemical company model), bisphenol A epoxy acrylate, urethane dibasic acid esters.
Further, described oxygenant is one or more the mixing in benzoyl peroxide, isopropyl benzene hydroperoxide, peroxidized t-butyl perbenzoate.
Further, described reductive agent is one or more the mixing in triethylamine, DMA, trolamine; The described reductive agent that helps is saccharin insoluble.
Further, described stopper is one or more the mixing in 1,4-naphthoquinone, Resorcinol, para benzoquinone.
Further, described coupling agent is (2,3-epoxypropyl) propyl trimethoxy silicane A-187.
Further, described surface promoter is one or more the mixing in ferrocene ethanolic soln, neutralized verdigris ethanolic soln, isocaprylic acid copper ethanolic soln, acetylacetone copper ethanolic soln.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of preparation method of sun power crystalline silicon rod splicing glue comprises the following steps:
(1) prepare respectively anaerobic gelatin and surface promoter:
1) be that the oligopolymer of 20～80 parts, the thinner of 10～30 parts, the stopper of 0.01～0.03 part add in stirrer and mix with parts by weight, add again parts by weight be 0.2～0.8 part reductive agent, 0.1～0.5 part help reductive agent, first heating, stir again, then the cooling room temperature of being down to, then to add parts by weight be the coupling agent of 1～5 part, again stirs, and then vacuumize, namely get the anaerobic gelatin of described sun power crystalline silicon rod splicing glue;
2) be the metal organic acid powder of 0.1～1 part with parts by weight, the solvent of 90～99.9 parts adds in stirrer and stirs, and to mixing, namely gets the surface promoter of described sun power crystalline silicon rod splicing glue.
When (2) using, will be dried, then be coated with anaerobic gelatin by the surperficial coated surfaces promotor of sticking crystalline silicon rod, dock namely bonding rapidly.Can locate about 10 seconds, carry out the wafer cutting after curing.
On the basis of technique scheme, the present invention can also do following improvement.
Further, in step 1) in, the temperature after described heating is 40～60 ℃.
Further, in step 1) in, the processing condition of described stirring are: be 500～1000 rev/mins at rotational velocity, revolution speed is under the condition of 5～8 rev/mins, to stir 0.3～1 hour.
Further, in step 1) in, the described time of again stirring is 0.5～1.5 hour; The described processing condition that vacuumize are: vacuumize 5～15 minutes, make vacuum tightness to-0.1～-0.08MPa.
Further, in step 2) in, the processing condition of described stirring are: be 200～500 rev/mins at rotational velocity, revolution speed is under the condition of 5～8 rev/mins, to stir 0.2～1 hour.
The invention has the beneficial effects as follows: sun power crystalline silicon rod splicing glue of the present invention has enough intensity to avoid under the prerequisite of quality accident in guaranteeing wafer cutting processing process, compare conventional epoxies glue, workpiece setting time be can obviously improve, bonding strength and toughness improved, improve stability in storage, technological operation and resistant to chemical media, reduce the moisture-sensitive degree of environment.
Embodiment
Below principle of the present invention and feature are described, example only be used for to be explained the present invention, is not be used to limiting scope of the present invention.
Embodiment 1
accurately take following various raw material: 67 parts of ethoxyquin bisphenol a dimethacrylate, 15 parts of the many acrylate of tetraethylene-glycol, 1, 0.02 part of 4-naphthoquinones adds in double-planet dynamic mixing stirrer and mixes, add again N, 0.5 part of accelerine, 0.3 part, asccharin, be warming up to 40 ℃, it is 500 rev/mins at described double-planet dynamic mixing stirrer rotational velocity, revolution speed is under the condition of 8 rev/mins, mechanical stirring made dissolving fully in 0.5 hour, the quick cooling room temperature of being down to subsequently, add 3 parts of benzoyl peroxides, add again 2 parts of A-187 coupling agents, stir 1 hour evenly after, vacuumize 10 minutes, vacuum tightness is to-0.1MPa.Discharging namely obtains the anaerobic gelatin that sun power crystalline silicon rod of the present invention splices, and packing is placed stand-by.
Accurately take each component of surface promoter as follows: be 0.2 part of isocaprylic acid copper powder with weight, 99.8 parts of solvents of dehydrated alcohol, add in double-planet dynamic mixing stirrer and mix, it is 300 rev/mins at described double-planet dynamic mixing stirrer rotational velocity, revolution speed is under the condition of 5 rev/mins, mechanical stirring 0.5 hour, discharging, namely obtain the promotor of sun power crystalline silicon rod splicing glue of the present invention, packing is placed stand-by.
Embodiment 2
accurately take following various raw material: 60 parts of bisphenol A epoxy acrylates, 20 parts of ethoxyquin bisphenol a dimethacrylate, 10 parts of hydroxyethyl methylacrylates, 0.02 part of Resorcinol adds in double-planet dynamic mixing stirrer and mixes, add again 0.2 part of triethylamine, 0.1 part, asccharin, be warming up to 60 ℃, it is 500 rev/mins at described double-planet dynamic mixing stirrer rotational velocity, revolution speed is under the condition of 8 rev/mins, mechanical stirring made dissolving fully in 0.5 hour, the quick cooling room temperature of being down to subsequently, add 2 parts of isopropyl benzene hydroperoxides, add again 1 part of A-187 coupling agent, stir 1 hour evenly after, vacuumize 10 minutes, vacuum tightness is to-0.08MPa.Discharging namely obtains the anaerobic gelatin that sun power crystalline silicon rod of the present invention splices, and packing is placed stand-by.
Accurately take each component of surface promoter as follows: be 0.8 part of butyl ferrocene with weight, 99.2 parts of solvents of dehydrated alcohol, add in double-planet dynamic mixing stirrer and mix, it is 300 rev/mins at described double-planet dynamic mixing stirrer rotational velocity, revolution speed is under the condition of 5 rev/mins, mechanical stirring 0.5 hour, discharging, namely obtain the promotor of sun power crystalline silicon rod splicing glue of the present invention, packing is placed stand-by.
Embodiment 3
accurately take following various raw material: 10 parts of ethoxyquin bisphenol a dimethacrylate, 20 parts of polyurethane-modified acrylic acid dibasic acid esters, 30 parts of 2-phenoxyethyl acrylate, 0.01 part of para benzoquinone adds in double-planet dynamic mixing stirrer and mixes, add again 0.8 part of trolamine, 0.5 part, asccharin, be warming up to 50 ℃, it is 500 rev/mins at described double-planet dynamic mixing stirrer rotational velocity, revolution speed is under the condition of 8 rev/mins, mechanical stirring made dissolving fully in 0.5 hour, the quick cooling room temperature of being down to subsequently, add 1 part of peroxidized t-butyl perbenzoate, add again 4 parts of A-187 coupling agents, stir 1 hour evenly after, vacuumize 10 minutes, vacuum tightness is to-0.06MPa.Discharging namely obtains the anaerobic gelatin that sun power crystalline silicon rod of the present invention splices, and packing is placed stand-by.
Accurately take each component of surface promoter as follows: be 1 part of neutralized verdigris powder with weight, 99 parts of solvents of dehydrated alcohol, add in double-planet dynamic mixing stirrer and mix, it is 300 rev/mins at described double-planet dynamic mixing stirrer rotational velocity, revolution speed is under the condition of 5 rev/mins, mechanical stirring 0.5 hour, discharging, namely obtain the promotor of sun power crystalline silicon rod splicing glue of the present invention, packing is placed stand-by.
Embodiment 4
accurately take following various raw material: 80 parts of bisphenol A epoxy acrylates, 20 parts of 2-phenoxyethyl acrylate, 1, 0.03 part of 4-naphthoquinones adds in double-planet dynamic mixing stirrer and mixes, add again 0.6 part of triethylamine, 0.4 part, asccharin, be warming up to 45 ℃, it is 500 rev/mins at described double-planet dynamic mixing stirrer rotational velocity, revolution speed is under the condition of 8 rev/mins, mechanical stirring made dissolving fully in 0.5 hour, the quick cooling room temperature of being down to subsequently, add 5 parts of isopropyl benzene hydroperoxides, add again 5 parts of A-187 coupling agents, stir 1 hour evenly after, vacuumize 10 minutes, vacuum tightness is to-0.05MPa.Discharging namely obtains the anaerobic gelatin that sun power crystalline silicon rod of the present invention splices, and packing is placed stand-by.
Accurately take each component of surface promoter as follows: be 0.6 part of methyl ethyl diketone copper powder with weight, 99.4 parts of solvents of dehydrated alcohol, add in double-planet dynamic mixing stirrer and mix, it is 300 rev/mins at described double-planet dynamic mixing stirrer rotational velocity, revolution speed is under the condition of 5 rev/mins, mechanical stirring 0.5 hour, discharging, namely obtain the promotor of sun power crystalline silicon rod splicing glue of the present invention, packing is placed stand-by.
Above embodiment 1 to embodiment 4 when technique is used, will be dried, then be coated with anaerobic gelatin by the surface of sticking crystalline silicon rod coating promotor, docking, and bonding, solidify the location, namely carries out the wafer cutting.
The comparative example 1
the conventional epoxies adhesive formulation, accurately take following various raw material: 55 parts of bisphenol A type epoxy resins, epoxy resin toughened 20 parts of end carboxyl nitrile rubber CTBN, 20 parts of active micro silicon powders, 3 parts of nano-calcium carbonates, 2 parts of aerosils, 0.2 part of KH-560 coupling agent, above-mentioned each raw material is added in double-planet dynamic mixing stirrer successively, be evacuated to-0.1MPa, it is 1000 rev/mins in rotational velocity, revolution speed is under the condition of 8 rev/mins, mechanical stirring 2 hours, mix, obtain the A component of epoxyn, packing is placed stand-by.
Accurately take each component of solidifying agent as follows: 65 parts of GPM800 epoxy hardeners, 13 parts of 650# polyamide curing agents, 22 parts, calcium carbonate adds above-mentioned each raw material in double-planet dynamic mixing stirrer successively, is evacuated to-0.1MPa, it is 1000 rev/mins in rotational velocity, revolution speed is that under the condition of 8 rev/mins, mechanical stirring 2 hours mixes, obtain the B component of epoxyn, packing is placed stand-by.
A component and the B component of the epoxyn that comparative example 1 is obtained took in 1: 1 by weight ratio, mix, and coating, solidify the location, then carry out the wafer cutting.
Performance by following experimental test sun power crystalline silicon rod splicing of the present invention glue.
The step of testing method is:
With the sun power crystalline silicon rod splicing glue that obtains in embodiment 1 to 4 each embodiment, when test, with the surface coating promotor of adherend, dry, then be coated with anaerobic gelatin 8-10 gram, docking, the location is solidified, then is carried out performance test.
A component and the B component of the epoxyn that comparative example 1 is obtained were mixed in 1: 1 by weight ratio, took mixed glue 8-10 gram, docking, and the location is solidified, then is carried out performance test.
The test of experimental example 1 shearing resistance:
Above-described embodiment 1-4 and existing conventional epoxies tackiness agent are compared test, test according to standard GB/T 6329-1996.
Experimental example 2 shock strength tests:
Above-described embodiment 1-4 and existing conventional epoxies tackiness agent are compared test, test according to standard GB/T 2571-1995.
The test of 3 setting times of experimental example:
Above-described embodiment 1-4 and existing conventional epoxies tackiness agent are compared test, test according to standard A STM 5363-1997.With the steel M8 screw bolt and nut after the acetone oil removing as the room temperature tested object.
Experimental example 4 stable storing property testings
Component with above-described embodiment 1-4 and existing conventional epoxies tackiness agent, respectively get 100g and pour in 200 milliliters of glass beakers, then be placed in climatic chamber, in the environment of 25 ℃ of temperature, relative humidity 50%, the glue changing condition is observed in uncovered placement 15 days.
Experimental example 5 medium-resistance tests
The component of above-described embodiment 1-4 and existing conventional epoxies tackiness agent is carried out bonding M10 bloom by institute's provisioning request, behind the location, room temperature was placed 24 hours, under 70 ℃ of conditions, soaked 24 hours in the 200# solvent oil respectively, test its compression shear strength, testing standard ginseng Q/SH 114-2009 standard is carried out.
The test acquired results as shown in Table 1.
Table one test acquired results
Can find out from the above results, a kind of sun power crystalline silicon rod splicing glue of the present invention is better than the mechanical property of existing conventional epoxies glue, and especially toughness is higher, and has improved simultaneously stability in storage and chemical mediator-resitant property.And neoteric silicon rod splicing glue is more quick setting time, has improved greatly work efficiency, can satisfy the requirement of positioning bonding fast in sun power crystal silicon cutting action fully.
The above is only preferred embodiment of the present invention, and is in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, is equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (10)
1. a sun power crystalline silicon rod splicing glue, is characterized in that, is comprised of anaerobic gelatin and promotor;
Wherein, described anaerobic gelatin is comprised of each raw material of following parts by weight: 10 ~ 30 parts of thinners, and 20 ~ 80 parts of oligopolymers, 1 ~ 5 part of coupling agent, 1 ~ 5 part, oxygenant, 0.2 ~ 0.8 part of reductive agent helps 0.1 ~ 0.5 part of reductive agent, 0.01 ~ 0.03 part of stopper;
Described surface promoter is comprised of each raw material of following parts by weight: 0.1 ~ 1 part of metal organic acid salt, 90 ~ 99.9 parts of solvents.
2. sun power crystalline silicon rod splicing glue according to claim 1, is characterized in that, described thinner is a kind of or several mixing arbitrarily in the many acrylate of tetraethylene-glycol, hydroxyethyl methylacrylate, 2-phenoxyethyl acrylate.
3. sun power crystalline silicon rod splicing glue according to claim 1, is characterized in that, described oligopolymer is a kind of or several mixing arbitrarily in ethoxyquin bisphenol a dimethacrylate, bisphenol A epoxy acrylate, urethane dibasic acid esters.
4. sun power crystalline silicon rod splicing glue according to claim 1, is characterized in that, described coupling agent is (2,3-epoxypropyl) propyl trimethoxy silicane; Described oxygenant is a kind of or several mixing arbitrarily in benzoyl peroxide, isopropyl benzene hydroperoxide, peroxidized t-butyl perbenzoate; Described reductive agent is a kind of or several mixing arbitrarily in triethylamine, DMA, trolamine; The described reductive agent that helps is saccharin insoluble; Described stopper is 1,4-naphthoquinone or Resorcinol.
5. sun power crystalline silicon rod splicing glue according to claim 1, is characterized in that, described surface promoter is a kind of or several mixing arbitrarily in ferrocene ethanolic soln, neutralized verdigris ethanolic soln, isocaprylic acid copper ethanolic soln.
6. the preparation method of a sun power crystalline silicon rod splicing glue, is characterized in that, comprises the following steps:
1) preparation process of the anaerobic gelatin of described sun power crystalline silicon rod splicing glue is: be that the oligopolymer of 20～80 parts, the thinner of 10～30 parts, the stopper of 0.01～0.03 part add in stirrer and mix with parts by weight, add again parts by weight be 0.2～0.8 part reductive agent, 0.1～0.5 part help reductive agent, first heating, stir again, then the cooling room temperature of being down to, adding parts by weight is the coupling agent of 1～5 part again, again stir, and then vacuumize, namely get the anaerobic gelatin of described sun power crystalline silicon rod splicing glue;
2) preparation process of the surface promoter of described sun power crystalline silicon rod splicing glue is: be the metal organic acid powder of 0.1～1 part with parts by weight, the solvent of 90～99.9 parts, add in stirrer and stir, to mixing, namely get the surface promoter of described sun power crystalline silicon rod splicing glue.
7. preparation method according to claim 6, is characterized in that, in step 1), the temperature after described heating is 40～60 ℃.
8. preparation method according to claim 6, is characterized in that, in step 1), the processing condition of described stirring are: be 500～1000 rev/mins at rotational velocity, revolution speed is under the condition of 5～8 rev/mins, to stir 0.3～1 hour.
9. preparation method according to claim 6, is characterized in that, in step 1), the described time of again stirring is 0.5～1.5 hour; The described processing condition that vacuumize are: vacuumize 5～15 minutes, make vacuum tightness to-0.1～-0.08MPa.
10. preparation method according to claim 6, is characterized in that, in step 2) in, the processing condition of described stirring are: be 200～500 rev/mins at rotational velocity, revolution speed is under the condition of 5～8 rev/mins, to stir 0.2～1 hour.
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| CN103555252A (en) * | 2013-10-23 | 2014-02-05 | 南宁珀源化工有限公司 | Fixing adhesive for cutting ceramic glass |
| CN104327775A (en) * | 2014-10-17 | 2015-02-04 | 太仓市茜泾化工有限公司 | UV (ultraviolet) curable adhesive and preparation method thereof |
| CN105001829A (en) * | 2015-07-02 | 2015-10-28 | 东莞优邦材料科技有限公司 | Priming coat type acrylic acid ester conductive adhesive and preparation method thereof |
| CN106590513A (en) * | 2016-10-31 | 2017-04-26 | 南宁珀源能源材料有限公司 | Powder silicon-ingot-cutting adhesive with good fluidity and preparation method thereof |
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| CN103319924A (en) * | 2013-07-05 | 2013-09-25 | 广东恒大新材料科技有限公司 | Anaerobic adhesive promoting primer and preparation method thereof |
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| CN103525356A (en) * | 2013-10-23 | 2014-01-22 | 南宁珀源化工有限公司 | Fixing glue for cutting sapphire |
| CN103555252A (en) * | 2013-10-23 | 2014-02-05 | 南宁珀源化工有限公司 | Fixing adhesive for cutting ceramic glass |
| CN103525356B (en) * | 2013-10-23 | 2015-04-15 | 南宁珀源化工有限公司 | Fixing glue for cutting sapphire |
| CN104327775A (en) * | 2014-10-17 | 2015-02-04 | 太仓市茜泾化工有限公司 | UV (ultraviolet) curable adhesive and preparation method thereof |
| CN105001829A (en) * | 2015-07-02 | 2015-10-28 | 东莞优邦材料科技有限公司 | Priming coat type acrylic acid ester conductive adhesive and preparation method thereof |
| CN105001829B (en) * | 2015-07-02 | 2018-01-05 | 东莞优邦材料科技股份有限公司 | A kind of primary coat type acrylate conductive adhesive and preparation method thereof |
| CN106590513A (en) * | 2016-10-31 | 2017-04-26 | 南宁珀源能源材料有限公司 | Powder silicon-ingot-cutting adhesive with good fluidity and preparation method thereof |
| CN106590513B (en) * | 2016-10-31 | 2019-09-20 | 南宁珀源能源材料有限公司 | Powder silicon ingot cutting glue of good fluidity and preparation method thereof |
| CN107189701A (en) * | 2017-07-03 | 2017-09-22 | 上海都伟光伏科技有限公司 | A kind of high temperature resistant anaerobism acrylic acid adhesive |
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