CN115232588B - Water boiling glue applied to large-size 210 silicon rod cutting and preparation method thereof - Google Patents

Water boiling glue applied to large-size 210 silicon rod cutting and preparation method thereof Download PDF

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Publication number
CN115232588B
CN115232588B CN202210783685.6A CN202210783685A CN115232588B CN 115232588 B CN115232588 B CN 115232588B CN 202210783685 A CN202210783685 A CN 202210783685A CN 115232588 B CN115232588 B CN 115232588B
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parts
component
stirring
degummed
settling agent
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CN115232588A (en
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赵含
刘远立
李世颖
高满
郭颂
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Guilin University of Technology
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Guilin University of Technology
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J163/00Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G59/00Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
    • C08G59/18Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
    • C08G59/40Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
    • C08G59/50Amines
    • C08G59/504Amines containing an atom other than nitrogen belonging to the amine group, carbon and hydrogen
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/02Non-macromolecular additives
    • C09J11/04Non-macromolecular additives inorganic
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/28Nitrogen-containing compounds
    • C08K2003/287Calcium, strontium or barium nitrates

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses a stick adhesive for large-size 210 cutting water boiling degumming and a preparation method thereof, and the stick adhesive mainly comprises the following components: the component A comprises 40-60 parts of epoxy resin, 1-10 parts of diluent, 0.1-1 part of anti-settling agent, 0.01-3 parts of defoamer and 40-60 parts of degummed inorganic substance; and the component B comprises the following components: the epoxy modified polyether amine curing agent comprises 10-40 parts of epoxy modified polyether amine curing agent, 20-30 parts of polythiol, 5-20 parts of accelerator, 30-70 parts of filler, 0.05-2 parts of defoamer and 0.05-5 parts of anti-settling agent. The product thus obtained not only ensures that the silicon rod with large size is cut without falling off the rod or the sheet, but also can be degummed under the condition of boiling. The invention is fast cured at low temperature, has stronger bonding strength, can be fast degummed in hot water with a certain temperature, avoids the defect of adding lactic acid in the degummed process, protects the environment, omits a sewage treatment part, and is beneficial to the health of operators.

Description

Water boiling glue applied to large-size 210 silicon rod cutting and preparation method thereof
Technical Field
The invention relates to the field of photovoltaic cutting adhesives, in particular to a glue stick applicable to large-size 210-size water-boiling degumming and a preparation method thereof.
Technical Field
In recent years, the solar photovoltaic industry develops rapidly, the market demand of clean energy will continue to expand, the share of solar energy generated energy will increase, so the demand of silicon wafers in the field will continue to increase, and the cutting of silicon wafers belongs to the upstream technology of solar cell production, and the quality and degumming in the cutting process will affect the conversion rate, yield, pollution rate and the like of the cell.
The cutting of the large size 210 nowadays, although the contact area becomes larger, the influence of the quality change is larger, so that higher requirements are put on the cohesiveness of the silicon rod; at present, the traditional degumming mode is not friendly to the environment due to the fact that lactic acid is used for degumming; in addition, the requirement for degumming is also higher because of the higher adhesiveness in order to obtain a silicon wafer with better quality.
Therefore, the hot-water degummed stick adhesive suitable for cutting the large-size 210 silicon rod has good adhesive property, and does not drop the rod or the sheet; can degumm in warm water at 50 ℃, ensures higher yield and lower pollution sheet rate, and is friendly to the environment.
Disclosure of Invention
The invention aims to provide the adhesive applied to cutting of the large-size silicon rod, which has higher adhesive property and certain toughness, and the risks of rod falling and sheet falling can not occur in the cutting process; the component A can be removed in warm water, and the selected inorganic degumming filler can be used as a filler, so that the cost is reduced, the solubility is higher under the condition of 50 ℃ in the degumming process, the better degumming effect is ensured, the higher yield in the degumming process is ensured, the pollution sheet rate can be reduced by hot water degumming, and the environment is also protected.
To achieve and other advantages in accordance with the purpose of the present invention, there is provided a stick adhesive for large-size cutting water-boiling degumming, comprising:
a component a comprising an epoxy resin; benzyl glycidyl ether; an anti-settling agent; a defoaming agent; degummed inorganic substances, and the like.
And the component B comprises the following components: it includes epoxy modified polyetheramines; modified polythiols; an accelerator; a filler; anti-settling agents, and the like.
Preferably comprises the following raw materials in parts by weight:
the component A comprises 58 parts of epoxy resin E51, 8 parts of benzyl glycidyl ether, 0.12 part of anti-settling agent, 0.05 part of defoamer and 42 parts of degummed inorganic substance; and the component B comprises the following components: the epoxy modified polyether amine curing agent comprises 40 parts of epoxy modified polyether amine curing agent, 6 parts of modified polythiol, 10 parts of accelerator, 54 parts of filler and 0.5 part of anti-settling agent.
Preferably, the epoxy resin in the component A is epoxy resin E-51 or E-44, the filler is calcium carbonate, the diluent is benzyl glycidyl ether, the anti-settling agent is fumed silica, the defoaming agent is BYK-322, and the degummed inorganic calcium nitrate.
Preferably, the epoxy modified polyether amine curing agent in the component B, the polythiol is polythiol QE-340M, the accelerator is K54, the filler is calcium carbonate, the defoamer is BYK-322, and the anti-settling agent is fumed silica.
Preferably, the preparation method of the glue stick capable of being degummed by boiling water comprises the following steps:
1. mixing 58 parts of epoxy resin E-51, 8 parts of benzyl glycidyl ether, 0.12 part of anti-settling agent fumed silica and 0.05 part of defoamer BYK-322 for 30min, adding 42 parts of calcium nitrate, stirring at a temperature not higher than 50 ℃ for 30min, and vacuumizing in a vacuum machine with a vacuum degree of 0.09MPa to obtain a component A;
2. the modified polyether amine curing agent is prepared by adding 40 parts of modified polyether amine curing agent QE-340M, 6 parts of modified polythiol, 54 parts of accelerator K, 10 parts of accelerator K, stirring for 30min, adding 54 parts of filler calcium carbonate, 0.5 part of anti-settling agent fumed silica, and stirring for 45 min. Vacuum pumping in a vacuum machine with the vacuum degree of 0.09MPa to obtain the component B.
Preferably, the A component and the B component are uniformly stirred according to the proportion of 1:1 when in use.
The invention at least comprises the following beneficial effects:
1. aiming at the large-size 210 silicon rod cutting, a certain proportion of amine curing agent is adopted, so that the adhesive force is improved, certain toughness is realized, meanwhile, the low shrinkage is ensured, and the risks of falling sheets, falling rods and the like in the cutting process are prevented.
2. In the silicon wafer cutting process, if lactic acid is used in the degumming process, the sewage aftertreatment is not only troublesome, but also sodium metasilicate is generated under the action of acid conditions and microorganisms, so that the sewage wafer rate is increased. The invention adopts warm water for degumming, which not only protects the environment, is beneficial to the health of workers, but also reduces the pollution rate to a certain extent.
3. Because the solubility of calcium nitrate in the inorganic filler is larger at 50 ℃, the price is low, and the inorganic filler has certain solubility in warm water after cutting is finished, and the degumming is faster. Therefore, the edge breakage rate is effectively reduced, and the yield of the slices is improved.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Detailed Description
The following detailed description of the invention, taken in conjunction with the examples, is provided to enable those skilled in the art to practice the invention by reference to the specification.
The experimental methods described in the following embodiments are conventional methods unless otherwise indicated, and the reagents and materials are commercially available.
< example 1>:
the glue stick glue capable of being degummed by boiling water comprises the following raw materials in parts by weight:
58 parts of A-component epoxy resin E-51, 8 parts of benzyl glycidyl ether, 0.12 part of anti-settling agent fumed silica, 0.05 part of defoamer BYK-322 and 42 parts of calcium nitrate.
The component B comprises 40 parts of modified polyether amine curing agent QE-340M, 6 parts of modified polythiol, 54 parts of accelerator K54, 54 parts of filler calcium carbonate and 0.5 part of anti-settling agent fumed silica.
The preparation method comprises the following steps:
adding 58 parts of epoxy resin E-51 parts, 8 parts of benzyl glycidyl ether, 0.12 part of anti-settling agent fumed silica, 0.05 part of defoamer BYK-322, stirring for 30min, then adding 42 parts of calcium nitrate, stirring uniformly at a rotating speed of 800rmp/min for 30min, and then placing into a vacuum machine with a vacuum degree of 0.09MPa for vacuumizing to obtain a component A;
adding 40 parts of modified polyether amine curing agent QE-340M, 6 parts of modified polythiol, 10 parts of accelerator K, stirring for 30min, adding 54 parts of filler calcium carbonate, 0.5 part of anti-settling agent fumed silica, and stirring for 45 min. Vacuum pumping in a vacuum machine with the vacuum degree of 0.09MPa to obtain the component B.
When in use, the component A and the component B are uniformly stirred according to the proportion of 1:1, and are coated on the surfaces of two objects to be pasted, and the two objects are butted.
< example 2>:
the glue stick glue capable of being degummed by boiling water comprises the following raw materials in parts by weight:
60 parts of epoxy resin E-51 parts of component A, 8 parts of benzyl glycidyl ether, 0.12 part of fumed silica as an anti-settling agent, 0.05 part of BYK-322 as an antifoaming agent and 40 parts of calcium nitrate.
The component B comprises 50 parts of modified polyether amine curing agent QE-340M, 2 parts of modified polythiol, 54 parts of accelerator K54, 48 parts of filler calcium carbonate and 0.6 part of anti-settling agent fumed silica.
The preparation method comprises the following steps:
adding 60 parts of epoxy resin E-51 parts, 8 parts of benzyl glycidyl ether, 0.12 part of anti-settling agent fumed silica, 0.05 part of defoamer BYK-322, stirring for 30min, then adding 40 parts of calcium nitrate, stirring uniformly at a rotating speed of 800rmp/min for 30min, and then placing into a vacuum machine with a vacuum degree of 0.09MPa for vacuumizing to obtain a component A;
50 parts of modified polyether amine curing agent QE-340M, 2 parts of modified polythiol, 54 parts of accelerator K, 48 parts of filler calcium carbonate and 0.6 part of anti-settling agent fumed silica are added into a stirring kettle, and stirring is carried out for 30min, thus obtaining the modified polyether amine curing agent. Vacuum pumping in a vacuum machine with the vacuum degree of 0.09MPa to obtain the component B.
When in use, the component A and the component B are uniformly stirred according to the proportion of 1:1, and are coated on the surfaces of two objects to be pasted, and the two objects are butted.
< example 3>:
the glue stick glue capable of being degummed by boiling water comprises the following raw materials in parts by weight:
45 parts of epoxy resin E-51 parts of component A, 8 parts of benzyl glycidyl ether, 0.12 part of fumed silica as an anti-settling agent, 0.05 part of BYK-322 as an antifoaming agent and 55 parts of calcium nitrate.
The component B comprises 30 parts of modified polyether amine curing agent QE-340M, 3 parts of modified polythiol, 15 parts of accelerator K54, 67 parts of filler calcium carbonate and 0.2 part of anti-settling agent fumed silica.
When in use, the component A and the component B are uniformly stirred according to the proportion of 1:1, and are coated on the surfaces of two objects to be pasted, and the two objects are butted.
Comparative example 1:
60 parts of A-component epoxy resin E-51 parts, 8 parts of benzyl glycidyl ether, 0.12 part of anti-settling agent fumed silica, 0.05 part of defoamer BYK-322 and 40 parts of calcium carbonate.
The component B comprises 50 parts of modified polyether amine curing agent QE-340M, 2 parts of modified polythiol, 54 parts of accelerator K54, 48 parts of filler calcium carbonate and 0.6 part of anti-settling agent fumed silica.
The preparation method comprises the following steps:
adding 60 parts of epoxy resin E-51 parts, 8 parts of benzyl glycidyl ether, 0.12 part of anti-settling agent fumed silica, 0.05 part of defoamer BYK-322, stirring for 30min, then adding 40 parts of calcium carbonate, stirring uniformly at a rotating speed of 800rmp/min for 30min, and then placing into a vacuum machine with a vacuum degree of 0.09MPa for vacuumizing to obtain a component A;
50 parts of modified polyether amine curing agent QE-340M, 2 parts of modified polythiol, 54 parts of accelerator K, 48 parts of filler calcium carbonate and 0.6 part of anti-settling agent fumed silica are added into a stirring kettle, and stirring is carried out for 30min, thus obtaining the modified polyether amine curing agent. Vacuum pumping in a vacuum machine with the vacuum degree of 0.09MPa to obtain the component B.
When in use, the component A and the component B are uniformly stirred according to the proportion of 1:1, and are coated on the surfaces of two objects to be pasted, and the two objects are butted.
Comparative example 2:
the glue stick glue capable of being degummed by boiling water comprises the following raw materials in parts by weight:
60 parts of epoxy resin E-51 parts of component A, 8 parts of benzyl glycidyl ether, 0.12 part of fumed silica as an anti-settling agent, 0.05 part of BYK-322 as an antifoaming agent and 40 parts of calcium nitrate.
The component B comprises 50 parts of modified polyether amine curing agent QE-340M, 2 parts of modified polythiol, 54 parts of accelerator K54, 48 parts of filler calcium nitrate and 0.6 part of anti-settling agent fumed silica.
When in use, the component A and the component B are uniformly stirred according to the proportion of 1:1, and are coated on the surfaces of two objects to be pasted, and the two objects are butted.
The relevant data were tested by applying the adhesive stick product described in examples 1-4 to a silicone stick and a resin plate.
We can see that: the increased level of amine curing agent increases the shear strength, but decreases the flexibility.
Degumming performance:
from the above data, it was found that degumming can be completed within 10min at 50℃when 54 parts of the additive amount was added to the A-component. When the calcium nitrate is the whole component in the AB, the degumming is faster, and the risk of falling sheets exists, so that the addition amount of 42 parts can be used for more stable degumming.

Claims (1)

1. The glue stick capable of being boiled for degumming is characterized by comprising the following raw materials in parts by weight:
and (3) a component A: 58 parts of epoxy resin E-51, 8 parts of benzyl glycidyl ether, 0.12 part of anti-settling agent fumed silica, 0.05 part of defoamer BYK-322 and 42 parts of calcium nitrate;
and the component B comprises the following components: 40 parts of modified polyether amine curing agent QE-340M, 6 parts of modified polythiol, 5410 parts of accelerator K, 54 parts of filler calcium carbonate and 0.5 part of anti-settling agent fumed silica;
the preparation method of the glue stick capable of being boiled for degumming comprises the following steps:
s1, adding epoxy resin E-51, benzyl glycidyl ether, anti-settling agent fumed silica and defoamer BYK-322 into a stirring kettle A, stirring for 30min, then adding calcium nitrate, stirring for 30min at the rotating speed of 800rmp, uniformly mixing, and then placing into a vacuum machine for vacuumizing, wherein the vacuum degree is 0.09MPa, thus obtaining a component A;
s2, adding a modified polyether amine curing agent QE-340M, modified polythiol and an accelerator K54 into a stirring kettle B, stirring for 30min, then adding filler calcium carbonate and anti-settling agent fumed silica, continuously stirring for 45min, and then placing into a vacuum machine for vacuumizing, wherein the vacuum degree is 0.09MPa, so that a component B is obtained;
and S3, uniformly stirring the component A and the component B according to the proportion of 1:1 to obtain the glue stick capable of being degummed by water boiling.
CN202210783685.6A 2022-07-05 2022-07-05 Water boiling glue applied to large-size 210 silicon rod cutting and preparation method thereof Active CN115232588B (en)

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CN115232588B true CN115232588B (en) 2023-08-22

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102850980A (en) * 2012-07-25 2013-01-02 常州大学 Epoxy resin glue for silicon rod cutting and preparation method thereof
CN107938347A (en) * 2017-12-01 2018-04-20 安踏(中国)有限公司 The shaping solution manufacturing method and shaping clothes preparation process of one-pass molding clothes
CN109321185A (en) * 2018-10-12 2019-02-12 南宁珀源能源材料有限公司 Can boiling degumming bar glue and preparation method thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103409090B (en) * 2013-06-05 2015-01-14 武汉市科达云石护理材料有限公司 Epoxy caulk compound used in humid environment

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102850980A (en) * 2012-07-25 2013-01-02 常州大学 Epoxy resin glue for silicon rod cutting and preparation method thereof
CN107938347A (en) * 2017-12-01 2018-04-20 安踏(中国)有限公司 The shaping solution manufacturing method and shaping clothes preparation process of one-pass molding clothes
CN109321185A (en) * 2018-10-12 2019-02-12 南宁珀源能源材料有限公司 Can boiling degumming bar glue and preparation method thereof

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