CN103571411B - Dual-component epoxy resin adhesive for splicing silicon block or silicon rod and preparation method of dual-component epoxy resin adhesive - Google Patents

Dual-component epoxy resin adhesive for splicing silicon block or silicon rod and preparation method of dual-component epoxy resin adhesive Download PDF

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CN103571411B
CN103571411B CN201310016053.8A CN201310016053A CN103571411B CN 103571411 B CN103571411 B CN 103571411B CN 201310016053 A CN201310016053 A CN 201310016053A CN 103571411 B CN103571411 B CN 103571411B
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epoxy resin
bisphenol
component
silicon rod
type epoxy
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CN103571411A (en
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许期斌
张丽芳
杨丽燕
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Shanghai Yu Xin Mstar Technology Ltd
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Shanghai Dou Wei Photovoltaic Science And Technology Ltd
Shanghai Dou Wei Electronics Co Ltd
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Abstract

The invention discloses a dual-component epoxy resin adhesive for splicing a silicon block or a silicon rod and a preparation method of the dual-component epoxy resin adhesive. The dual-component epoxy resin adhesive for splicing the silicon block or the silicon rod consists of a component A and a component B in ratio of 1: 1, wherein the component A comprises the following materials by mass percent: 30 to 60% of epoxy resin, 10 to 30% of formaldehyde modified epoxy resin, 1 to 5% of thixotropic agent, and 20 to 50% of filling agent; and the component B comprises the following materials by mass percent: 20 to 50% of modified amine curing agent, 10 to 40% of polymeric mercaptan, 3 to 5% of accelerant, 1 to 5% of thixotropic agent, and 20 to 60% of filling agent. By adopting the preparation method, the primary curing time is decreased, and the process requirements are met.

Description

For bicomponent epoxy resin glue that silico briquette or silicon rod splice and preparation method thereof
Technical field
The present invention relates to a kind of bicomponent epoxy resin glue and preparation method thereof, particularly relate to a kind of bicomponent epoxy resin glue and preparation method thereof for silico briquette or silicon rod splicing.
Background technology
In recent years, along with the rise of clean energy, solar photovoltaic industry is also started upsurge, the time domestic solar silicon wafers cutting enterprise of a few years surges to family more than 300 by tens, thus improve the usage quantity of various auxiliary material, and sizing agent is also one of indispensable auxiliary material in silicon chip cutting technique, different technique needs the sizing agent of different performance, wherein a kind of sizing agent is then need vertical surface to construct, high rigidity and the heat-resisting feature of height could meet its technique, because crystalline silicon is in growth, the number of charging capacity, the control of crystal diameter, the control of flavoring food all has an impact to the growth of crystal, thus produce the different silico briquette (silicon rod) of length, as follows to the method for the process of those stubs: one is again melted down, a kind of is the size adjusting wire-electrode cutting device, a kind of is connect silico briquette (silicon rod) different in size directly upper machine cutting with splicing.Two kinds of methods add loss above, consume the energy, increase cost, cause and bring very large inconvenience in silicon chip cutting; Same for this glue silico briquette (silicon rod) effectively, simply, directly together can be participated in cutting, thus ensure that the consistence of line cutting machine device parameter, simplify wire cutting technology by the latter's method.Now, sizing agent needs high thixotropic, the normal wire cutting technology of feature guarantee of high rigidity and thermotolerance to a certain degree.
Although also have this type of epoxy adhesive at present, but for reaching high rigidity and thermotolerance, then need heating cure or self-vulcanizing chronic, spelling sticklac as Lord Corp. of the U.S. needs heating cure, though the capable company in Hangzhou is self-vulcanizing, primary solidification just needs 1 ~ 2 hour, solidifies completely, needs more than 8 hours, this also brings very big inconvenience to pipelining, and pending thing packing phenomenon is obvious.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of bicomponent epoxy resin glue and preparation method thereof for silico briquette or silicon rod splicing, and it shortens the primary solidification time, while can meet processing requirement again.
The present invention solves above-mentioned technical problem by following technical proposals: a kind of bicomponent epoxy resin glue spliced for silico briquette or silicon rod, it is characterized in that, described for silico briquette or silicon rod splicing bicomponent epoxy resin glue by ratio be 1: 1 component A and B component form;
Component A is as follows, by mass percentage: epoxy resin 30 ~ 60%, and phenol aldehyde modified epoxy resin 10 ~ 30%, thixotropic agent 1 ~ 5%, weighting agent 20 ~ 50%;
B component is as follows, by mass percentage: modified amine curing agent 20 ~ 50%, and polymerization mercaptan 10 ~ 40%, promotor 3 ~ 5%, thixotropic agent 1 ~ 5%, weighting agent 20 ~ 60%.
Preferably, described epoxy resin is bisphenol A type epoxy resin or bisphenol f type epoxy resin.
Preferably, the bisphenol A type epoxy resin that the bisphenol A type epoxy resin that described bisphenol A type epoxy resin comprises bisphenol A type epoxy resin that oxirane value is 0.44mol/100g, oxirane value is 0.51mol/100g, oxirane value are 0.54mol/100g, oxirane value are the bisphenol A type epoxy resin of 0.55mol/100g, oxirane value is any one or more than one mixture in the bisphenol A type epoxy resin of 0.56mol/100g, the bisphenol f type epoxy resin of bisphenol f type epoxy resin to be oxirane value be 0.55 ~ 0.62mol/100g.
Preferably, the mixture that described phenol aldehyde modified epoxy resin comprises novolac epoxy that oxirane value is 0.47 ~ 0.51mol/100g, oxirane value is the o-cresol formaldehyde epoxy resin any one or more than one of 0.45 ~ 0.51mol/100g.
Preferably, described thixotropic agent is the mixture of gas phase sio2, attapulgite, wilkinite, organobentonite any one or more than one.
Preferably, described weighting agent is silicon powder, active micro silicon powder, kaolin, ultrafine kaolin, one or more mixtures of silica powder.
Preferably, described modified amine curing agent comprises phenol aldehyde modified aliphatic amide, phenol aldehyde modified aliphatic cyclic amine, one or more mixtures of modification aliphatic cyclic amine.
Preferably, described polymerization mercaptan comprises on-catalytic mercaptan, pre-catalyze thiol or epoxy toughess at room temperature.
Preferably, described promotor comprises 2,4,6-tri-(dimethylamino methyl), meta-cresol, Resorcinol, phenol.
The present invention also provides a kind of preparation method of bicomponent epoxy resin glue for silico briquette or silicon rod splicing, it is characterized in that, described preparation method adopts the bicomponent epoxy resin glue as above for silico briquette or silicon rod splicing, and described preparation method comprises the steps:
Process prepared by component A is as follows: by epoxy resin, phenol aldehyde modified epoxy resin, thixotropic agent, and weighting agent is fed in reactor, vacuum stirring 1.5 ~ 3 hours;
Process prepared by B component is as follows: by modified amine curing agent, polymerization mercaptan, promotor, thixotropic agent, and weighting agent drops in reactor, vacuum stirring 1.5 ~ 3 hours.
Positive progressive effect of the present invention is: the present invention adopt polymerization mercaptan and modified amine curing agent composite, in the presence of basic-type accelerator, the thiolate ion that thiol group generates and epoxy reaction, this speed of reaction is very fast, therefore can shorten the primary solidification time through the collocation of polymerization mercaptan and promotor.The present invention shortens the primary solidification time, can meet processing requirement again simultaneously.Vertical surface application property of the present invention is convenient, and cured article hardness is high, and thermotolerance is high, can not produce steel wire breakage during cutting.Component A and B component, after mixing under room temperature, are applied in ready silico briquette (silicon rod) vertical surface, two pieces of silico briquettes (silicon rod) are vertically fixed, 15 ~ 45 minutes setting times, can cut after 3 ~ 8 hours.
Embodiment
The present invention be used for silico briquette or silicon rod splicing bicomponent epoxy resin glue by ratio be 1: 1 component A and B component form;
Component A is as follows, by mass percentage: epoxy resin 30 ~ 60%, and phenol aldehyde modified epoxy resin 10 ~ 30%, thixotropic agent 1 ~ 5%, weighting agent 20 ~ 50%;
B component is as follows, by mass percentage: modified amine curing agent 20 ~ 50%, and polymerization mercaptan 10 ~ 40%, promotor 3 ~ 5%, thixotropic agent 1 ~ 5%, weighting agent 20 ~ 60%.
Wherein, epoxy resin is bisphenol A type epoxy resin or bisphenol f type epoxy resin.The bisphenol A type epoxy resin that the bisphenol A type epoxy resin that bisphenol A type epoxy resin comprises bisphenol A type epoxy resin that oxirane value is 0.44mol/100g, oxirane value is 0.51mol/100g, oxirane value are 0.54mol/100g, oxirane value are the bisphenol A type epoxy resin of 0.55mol/100g, oxirane value is any one or more than one mixture in the bisphenol A type epoxy resin of 0.56mol/100g, the bisphenol f type epoxy resin of bisphenol f type epoxy resin to be oxirane value be 0.55 ~ 0.62mol/100g.The mixture that phenol aldehyde modified epoxy resin comprises novolac epoxy that oxirane value is 0.47 ~ 0.51mol/100g, oxirane value is the o-cresol formaldehyde epoxy resin any one or more than one of 0.45 ~ 0.51mol/100g.Thixotropic agent is the mixture of gas phase sio2, attapulgite, wilkinite, organobentonite any one or more than one.Weighting agent is silicon powder, active micro silicon powder, kaolin, ultrafine kaolin, one or more mixtures of silica powder.Modified amine curing agent comprises phenol aldehyde modified aliphatic amide, phenol aldehyde modified aliphatic cyclic amine, one or more mixtures of modification aliphatic cyclic amine.Promotor comprises 2,4,6-tri-(dimethylamino methyl), meta-cresol, Resorcinol, phenol.Described polymerization mercaptan comprises on-catalytic mercaptan, pre-catalyze thiol or epoxy toughess at room temperature, specifically comprise following type product: Capcure3-800 (the peaceful on-catalytic mercaptan of section), Capcure3830-81 (the peaceful 3830-81 of section), Capcure40secHV (the peaceful pre-catalyze thiol of section), CapcureLOF (the peaceful on-catalytic mercaptan of section), Capcure WR-6 (pre-catalyze thiol), Epomate QX-lO (epoxy toughess at room temperature), EPomate qx-40 (epoxy toughess at room temperature), MP-gg90 (Polymercaptan curing agent), EH-316 (Polymercaptan curing agent), EH-317 (Polymercaptan curing agent, Japan's trade mark).
The preparation method of bicomponent epoxy resin glue for silico briquette or silicon rod splicing comprises the steps:
Process prepared by component A is as follows: by epoxy resin, phenol aldehyde modified epoxy resin, thixotropic agent, and weighting agent is fed in reactor, vacuum stirring 1.5 ~ 3 hours;
Process prepared by B component is as follows: by modified amine curing agent, polymerization mercaptan, promotor, thixotropic agent, and weighting agent drops in reactor, vacuum stirring 1.5 ~ 3 hours.
Embodiment 1
Prepared by component A: epoxy resin, phenol aldehyde modified epoxy resin, gas phase sio2, silicon powder are fed into by mass percentage in reactor, vacuum stirring 1.5 hours.
Prepared by B component: by phenol aldehyde modified aliphatic amide, polymerization mercaptan, 2,4,6-tri-(dimethylamino methyl), gas phase sio2, silicon powder drops in reactor by mass percentage, vacuum stirring 1.5 hours.
Embodiment 2
Process prepared by component A is as follows: epoxy resin, phenol aldehyde modified epoxy resin, wilkinite, silicon powder are fed into by mass percentage in reactor, vacuum stirring 3 hours.
Process prepared by B component is as follows: by phenol aldehyde modified aliphatic amide, polymerization mercaptan, 2,4,6-tri-(dimethylamino methyls), gas phase sio2, silicon powder drops in reactor by mass percentage, vacuum stirring 3 hours.
Embodiment 3
Process prepared by component A is as follows: epoxy resin, phenol aldehyde modified epoxy resin, wilkinite, silicon powder are fed into by mass percentage in reactor, vacuum stirring 3 hours.
Process prepared by B component is as follows: by phenol aldehyde modified aliphatic amide, polymerization mercaptan, 2,4,6-tri-(dimethylamino methyls), wilkinite, silicon powder drops in reactor by mass percentage, vacuum stirring 3 hours.
Embodiment 4
Process prepared by component A is as follows: by epoxy resin, phenol aldehyde modified epoxy resin, gas phase SiO 2, kaolin is fed in reactor by mass percentage, vacuum stirring 3 hours.
Process prepared by B component is as follows: by phenol aldehyde modified aliphatic amide, polymerization mercaptan, 2,4,6-tri-(dimethylamino methyls), gas phase sio2, kaolin drops in reactor by mass percentage, vacuum stirring 3 hours.
The characteristic of bicomponent epoxy resin glue for silico briquette or silicon rod splicing is shown in table 1 (test condition: 25 DEG C, relative humidity 50%):
Table 1
Those skilled in the art can carry out various remodeling and change to the present invention.Therefore, present invention covers the various remodeling in the scope falling into appending claims and equivalent thereof and change.

Claims (6)

1. for a bicomponent epoxy resin glue for silico briquette or silicon rod splicing, it is characterized in that, the described bicomponent epoxy resin glue for silico briquette or silicon rod splicing is that the component A of 1:1 and B component form by ratio;
Component A is as follows, by mass percentage: epoxy resin 30 ~ 60%, and phenol aldehyde modified epoxy resin 10 ~ 30%, thixotropic agent 1 ~ 5%, weighting agent 20 ~ 50%;
B component is as follows, by mass percentage: modified amine curing agent 20 ~ 50%, and polymerization mercaptan 10 ~ 40%, promotor 3 ~ 5%, thixotropic agent 1 ~ 5%, weighting agent 20 ~ 60%.
2., as claimed in claim 1 for the bicomponent epoxy resin glue that silico briquette or silicon rod splice, it is characterized in that, described epoxy resin is bisphenol A type epoxy resin or bisphenol f type epoxy resin.
3. the bicomponent epoxy resin glue spliced for silico briquette or silicon rod as claimed in claim 2, it is characterized in that, described bisphenol A type epoxy resin comprises the bisphenol A type epoxy resin that oxirane value is 0.44mol/100g, oxirane value is the bisphenol A type epoxy resin of 0.51mol/100g, oxirane value is the bisphenol A type epoxy resin of 0.54 mol/100g, oxirane value is the bisphenol A type epoxy resin of 0.55 mol/100g, oxirane value is any one or more than one mixture in the bisphenol A type epoxy resin of 0.56 mol/100g, the bisphenol f type epoxy resin of bisphenol f type epoxy resin to be oxirane value be 0.55 ~ 0.62mol/100g.
4. the bicomponent epoxy resin glue spliced for silico briquette or silicon rod as claimed in claim 1, it is characterized in that, described phenol aldehyde modified epoxy resin comprises novolac epoxy that oxirane value is 0.47 ~ 0.51mol/100g, mixture that oxirane value is the o-cresol formaldehyde epoxy resin any one or more than one of 0.45 ~ 0.51 mol/100g.
5., as claimed in claim 1 for the bicomponent epoxy resin glue that silico briquette or silicon rod splice, it is characterized in that, described thixotropic agent is gas phase SiO 2, attapulgite, wilkinite, organobentonite any one or more than one mixture.
6. the preparation method of the bicomponent epoxy resin glue spliced for silico briquette or silicon rod, it is characterized in that, described preparation method adopts the bicomponent epoxy resin glue spliced for silico briquette or silicon rod according to any one of claim 1 to 5, and described preparation method comprises the steps:
Process prepared by component A is as follows: be fed in reactor by epoxy resin, phenol aldehyde modified epoxy resin, thixotropic agent, weighting agent, vacuum stirring 1.5 ~ 3 hours;
Process prepared by B component is as follows: drop in reactor by modified amine curing agent, polymerization mercaptan, promotor, thixotropic agent, weighting agent, vacuum stirring 1.5 ~ 3 hours.
CN201310016053.8A 2013-01-16 2013-01-16 Dual-component epoxy resin adhesive for splicing silicon block or silicon rod and preparation method of dual-component epoxy resin adhesive Active CN103571411B (en)

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CN105022119B (en) * 2015-08-07 2018-07-31 中时讯通信建设有限公司 A kind of optical fiber splicing method
CN106753130A (en) * 2016-12-23 2017-05-31 上海康达化工新材料股份有限公司 A kind of modified epoxy for diamond wire cutting silicon rod glue
CN112793021A (en) * 2019-10-28 2021-05-14 洛阳阿特斯光伏科技有限公司 Silicon rod splicing method, spliced silicon rod and cutting method of spliced silicon rod
CN112940658A (en) * 2021-02-01 2021-06-11 南宁珀源能源材料有限公司 Stick glue and preparation method and application thereof
CN112852367B (en) * 2021-03-08 2023-05-12 广西珀源新材料有限公司 Double-component silicon rod splicing adhesive and preparation method thereof
CN113604183A (en) * 2021-08-20 2021-11-05 杭州固安科技有限公司 Rigid epoxy glue solution
CN114276765A (en) * 2021-12-27 2022-04-05 句容协鑫光伏科技有限公司 Rod adhesive for improving cutting edge breakage rate of thin wire thin sheet large-size silicon rod and preparation method thereof
CN114921210A (en) * 2022-06-17 2022-08-19 宜春宇泽新能源有限公司 Adhesive for solar-grade silicon wafer suitable for large-size flaking and preparation process and use method thereof
CN117247756B (en) * 2023-08-23 2024-05-28 广东金湾高景太阳能科技有限公司 Silicon rod joint glue and preparation method and application thereof

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CN102120925A (en) * 2011-02-14 2011-07-13 上海康达化工新材料股份有限公司 Modified epoxy resin of monocrystalline silicon rod cutting glue and preparation method thereof
CN102627931A (en) * 2012-03-23 2012-08-08 烟台德邦科技有限公司 Pre-catalytic bonding glue and preparation method thereof

Patent Citations (2)

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CN102120925A (en) * 2011-02-14 2011-07-13 上海康达化工新材料股份有限公司 Modified epoxy resin of monocrystalline silicon rod cutting glue and preparation method thereof
CN102627931A (en) * 2012-03-23 2012-08-08 烟台德邦科技有限公司 Pre-catalytic bonding glue and preparation method thereof

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