CN114921210A - Adhesive for solar-grade silicon wafer suitable for large-size flaking and preparation process and use method thereof - Google Patents

Adhesive for solar-grade silicon wafer suitable for large-size flaking and preparation process and use method thereof Download PDF

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Publication number
CN114921210A
CN114921210A CN202210693142.5A CN202210693142A CN114921210A CN 114921210 A CN114921210 A CN 114921210A CN 202210693142 A CN202210693142 A CN 202210693142A CN 114921210 A CN114921210 A CN 114921210A
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parts
component
calcium carbonate
epoxy resin
fumed silica
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伍金军
胡建亮
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Yichun Yuze New Energy Co ltd
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Yichun Yuze New Energy Co ltd
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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
    • 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
    • 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
    • C09J11/06Non-macromolecular additives organic
    • 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
    • C08K3/18Oxygen-containing compounds, e.g. metal carbonyls
    • C08K3/24Acids; Salts thereof
    • C08K3/26Carbonates; Bicarbonates
    • C08K2003/265Calcium, strontium or barium carbonate
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50Manufacturing or production processes characterised by the final manufactured product

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  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Adhesives Or Adhesive Processes (AREA)

Abstract

The invention discloses a viscose adhesive for a large-size flaky solar-grade silicon wafer and a preparation process and a use method thereof, and the viscose adhesive comprises a component A and a component B; the component A comprises the following components in parts by weight: modified epoxy resin: 36-56 parts; low-viscosity phenolic-modified epoxy resin: 8-28 parts; benzyl glycidyl ether: 1-5 parts; calcium carbonate: 20-40 parts; white colorant: 0.5-4 parts; fumed silica: 0.05-0.4 part; the component B comprises the following components in parts by weight: polythiol: 50-70 parts; accelerator (b): 2-8 parts; epoxy reactive diluent: 0.5-4 parts; calcium carbonate: 20-35 parts; red colorant: 0.1-0.8 part; fumed silica: 0.02-0.3 part, reasonable structure, low collapse, high qualification rate, good anti-dropping effect, low thread hanging rate of a glue layer, low viscosity and high fluidity.

Description

Adhesive for solar-grade silicon wafer suitable for large-size flaking and preparation process and use method thereof
Technical Field
The invention relates to a viscose, in particular to a viscose for a large-size flaky solar-grade silicon wafer, and a preparation process and a use method thereof.
Background
At present, the mainstream size of silicon slice cutting in the photovoltaic solar industry is a single crystal silicon rod with the width of 182mm, the slice thickness of wire cutting is 160 micrometers and 170 micrometers, and the wire diameter of a used multi-wire cutting diamond wire is 38 micrometers and 40 micrometers; the conventional glue for sticking rods on the market only can cut specifications below 166 width and above 160 mu m in thickness due to relatively poor performances of a glue film such as heat resistance, adhesive force and the like, and develops towards the trend of thinning wire cutting and thin silicon wafers of large-size silicon wafers and diamond wires along with the continuous progress of the cutting technology of photovoltaic silicon rods and the requirements of cost reduction and efficiency improvement, the defect rate can be increased to be more than or equal to 5.6 percent by using the conventional glue for sticking the wafers with the width of more than 182mm or the thickness of below 160 mu m and corresponding to the wire cutting process with the wire diameter of below 40 mu m, the defect rate is continuously higher, and the qualified rate cannot meet the production requirements of enterprises.
In the prior art, when conventional viscose glue is used, the heat resistance, toughness and other properties of the conventional viscose glue cannot meet the requirements of a thin wire cutting and large size silicon rod flaking wire cutting process, so that the collapse is high and the yield is low. In addition, in the process of thinning and wire cutting of the large-size silicon rod by the fine-wire cutting method, the adhesive layer is subjected to external stress circulation wire cutting of the diamond wire, the adhesive layer is more easily damaged, so that the adhesive force between the adhesive layer and the silicon wafer is reduced, and the phenomenon of easy wafer falling is caused. In addition, the thickness of the adhesive layer cannot be well controlled, the thickness of the adhesive layer is not uniform, the phenomenon of thread hanging caused by thread cutting to the adhesive layer is easy to occur, the thread hanging rate of the adhesive layer is high, the viscosity is strong, and the fluidity is poor, so that the adhesive for the solar-grade silicon wafer suitable for large-size flaking is urgently needed to solve the problems.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a food-grade formula of a viscose adhesive for a large-size flaky solar-grade silicon wafer, a preparation process and a use method thereof, and aims to solve the problems in the background art.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a viscose adhesive for solar-grade silicon wafers applicable to large-size flaking comprises a component A and a component B;
the component A comprises the following components in parts by weight:
modified epoxy resin: 36-56 parts;
low-viscosity phenolic-modified epoxy resin: 8-28 parts;
benzyl glycidyl ether: 1-5 parts;
calcium carbonate: 20-40 parts;
white colorant: 0.5-4 parts;
fumed silica: 0.05-0.4 part;
the component B comprises the following components in parts by weight:
polythiol: 50-70 parts;
accelerator (b): 2-8 parts;
epoxy reactive diluent: 0.5-4 parts;
calcium carbonate: 20-35 parts;
red colorant: 0.1-0.8 part;
fumed silica: 0.02-0.3 portion.
The adhesive for the solar-grade silicon wafer suitable for large-size flaking is characterized by comprising a component A and a component B;
the component A comprises the following components in parts by weight:
modified epoxy resin: 46 parts of (a);
low-viscosity phenolic-modified epoxy resin: 18 parts of a mixture;
benzyl glycidyl ether: 3 parts of a mixture;
calcium carbonate: 30.8 parts;
white colorant: 2 parts of a mixture;
fumed silica: 0.2 part;
the component B comprises the following components in parts by weight:
polythiol: 64 parts;
accelerator (b): 5.8 parts;
epoxy reactive diluent: 2.2 parts of;
calcium carbonate: 27.5 parts;
red colorant: 0.4 part;
fumed silica: 0.1 part.
The adhesive for the solar-grade silicon wafer suitable for large-size flaking is characterized by comprising a component A and a component B;
the component A comprises the following components in parts by weight:
modified epoxy resin: 37 parts of;
low-viscosity phenolic-modified epoxy resin: 10 parts of a binder;
benzyl glycidyl ether: 2 parts of (1);
calcium carbonate: 30.8 parts;
white colorant: 2 parts of a mixture;
fumed silica: 0.2 part;
the component B comprises the following components in parts by weight:
polythiol: 50 parts of a mixture;
accelerator (b): 2 parts of (1);
epoxy reactive diluent: 0.6 part;
calcium carbonate: 27.5 parts;
red colorant: 0.4 part;
fumed silica: 0.1 part.
The adhesive for the solar-grade silicon wafer suitable for large-size flaking is characterized by comprising a component A and a component B;
the component A comprises the following components in parts by weight:
modified epoxy resin: 54 parts of a binder;
low-viscosity phenolic-modified epoxy resin: 24 parts of (1);
benzyl glycidyl ether: 4 parts of a mixture;
calcium carbonate: 30.8 parts;
white colorant: 2 parts of a mixture;
fumed silica: 0.2 part;
the component B comprises the following components in parts by weight:
polythiol: 68 parts of (b);
accelerator (b): 7 parts;
epoxy reactive diluent: 3.5 parts;
calcium carbonate: 27.5 parts;
red colorant: 0.4 part;
fumed silica: 0.1 part.
A preparation process of an adhesive for a large-size flaky solar-grade silicon wafer comprises the following steps,
step (A), preparing the component A, namely preparing the following components in parts by weight: modified epoxy resin: 36-56 parts; low-viscosity phenolic-modified epoxy resin: 8-28 parts; benzyl glycidyl ether: 1-5 parts; calcium carbonate: 20-40 parts; white colorant: 0.5-4 parts; fumed silica: 0.05-0.4 part;
step (B), sequentially adding the modified epoxy resin, the low-viscosity phenolic aldehyde modified epoxy resin, the benzyl glycidyl ether, the calcium carbonate, the white colorant and the gas-phase silica in the step (A) into a stirring cylinder, dispersing and stirring for 30-50min, grinding by a grinding machine until the fineness is less than 80 mu m, defoaming, filtering and packaging to obtain a component A;
step (C), preparing the component B, namely preparing the following components in parts by weight: polythiol: 50-70 parts; accelerator (b): 2-8 parts; epoxy reactive diluent: 0.5-4 parts; calcium carbonate: 20-35 parts; red colorant: 0.1-0.8 part; fumed silica: 0.02-0.3 part;
and (D) sequentially adding the polythiol, the accelerator, the epoxy active diluent, the calcium carbonate, the red colorant and the fumed silica in the step (C) into a stirring cylinder, dispersing and stirring for 35-55min, grinding by using a grinding machine until the fineness is less than 55 mu m, defoaming, filtering and packaging to obtain a component B.
The preparation process of the adhesive for the solar-grade silicon wafer suitable for large-size flaking is characterized in that the dispersing and stirring time in the step (C) is 40min, and the dispersing and stirring time in the step (D) is 45 min.
A method for using a viscose for a large-size flaky solar-grade silicon wafer is characterized in that a component A and a component B are uniformly mixed according to a mass ratio of 1: 1-1.2 for use.
In the application method of the adhesive for the solar-grade silicon wafer suitable for large-size flaking, the component A and the component B are uniformly mixed according to the mass ratio of 1: 1 for use.
The beneficial effects of the invention are: the invention relates to a viscose adhesive for a large-size flaky solar-grade silicon wafer and a preparation process and a use method thereof,
1. according to the invention, the modified epoxy resin and the low-viscosity phenolic aldehyde modified epoxy resin are used, so that the hardness of the adhesive film is increased, the TG of the adhesive film is improved, the heat resistance of the adhesive film is improved, the temperature rise of the adhesive film caused by the failure of heat to be taken away in time is resisted, the deformation of the adhesive film is reduced, the phenomena of sheet falling and high collapse rate of the adhesive surface of the silicon wafer caused by the reduction of the performance due to the damage of the adhesive layer are avoided, the sheet falling rate and the collapse rate are reduced, and the qualified rate is improved.
2. According to the invention, the viscosity of the adhesive is adjusted by adding benzyl glycidyl ether, the viscosity of the adhesive is reduced to be proper, the fluidity is improved, the thickness of the adhesive layer is controlled when a silicon rod is bonded, and the problem of thread hanging is solved, so that the thread hanging rate of the adhesive layer is reduced.
Detailed Description
The present invention is further described below. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
The invention relates to a viscose adhesive for a solar-grade silicon wafer applicable to large-size flaking, which comprises a component A and a component B;
the component A comprises the following components in parts by weight:
modified epoxy resin: 36-56 parts;
low-viscosity phenolic-modified epoxy resin: 8-28 parts;
benzyl glycidyl ether: 1-5 parts;
calcium carbonate: 20-40 parts;
white colorant: 0.5-4 parts;
fumed silica: 0.05-0.4 part;
the component B comprises the following components in parts by weight:
polythiol: 50-70 parts;
accelerator (b): 2-8 parts;
epoxy reactive diluent: 0.5-4 parts;
calcium carbonate: 20-35 parts;
red colorant: 0.1-0.8 part;
fumed silica: 0.02-0.3 portion.
The adhesive for the solar-grade silicon wafer suitable for large-size flaking is characterized by comprising a component A and a component B;
the component A comprises the following components in parts by weight:
modified epoxy resin: 46 parts of a catalyst;
low-viscosity phenolic-modified epoxy resin: 18 parts of a mixture;
benzyl glycidyl ether: 3 parts of a mixture;
calcium carbonate: 30.8 parts;
white colorant: 2 parts of (1);
fumed silica: 0.2 part;
the component B comprises the following components in parts by weight:
polythiol: 64 parts;
accelerator (b): 5.8 parts;
epoxy reactive diluent: 2.2 parts of;
calcium carbonate: 27.5 parts;
red colorant: 0.4 part;
fumed silica: 0.1 part.
The adhesive for the solar-grade silicon wafer suitable for large-size flaking is characterized by comprising a component A and a component B;
the component A comprises the following components in parts by weight:
modified epoxy resin: 37 parts of;
low-viscosity phenolic-modified epoxy resin: 10 parts of a binder;
benzyl glycidyl ether: 2 parts of (1);
calcium carbonate: 30.8 parts;
white colorant: 2 parts of (1);
fumed silica: 0.2 part;
the component B comprises the following components in parts by weight:
polythiol: 50 parts of a mixture;
accelerator (b): 2 parts of a mixture;
epoxy reactive diluent: 0.6 part;
calcium carbonate: 27.5 parts;
red colorant: 0.4 part;
fumed silica: 0.1 part.
The adhesive for the solar-grade silicon wafer suitable for large-size flaking is characterized by comprising a component A and a component B;
the component A comprises the following components in parts by weight:
modified epoxy resin: 54 parts of a binder;
low-viscosity phenolic-modified epoxy resin: 24 parts of (1);
benzyl glycidyl ether: 4 parts of a mixture;
calcium carbonate: 30.8 parts;
white colorant: 2 parts of a mixture;
fumed silica: 0.2 part;
the component B comprises the following components in parts by weight:
polythiol: 68 parts of a mixture;
accelerator (b): 7 parts;
epoxy reactive diluent: 3.5 parts;
calcium carbonate: 27.5 parts;
red colorant: 0.4 part;
fumed silica: 0.1 part.
A preparation process of an adhesive for a large-size flaky solar-grade silicon wafer comprises the following steps,
step (A), preparing the component A, namely preparing the following components in parts by weight: modified epoxy resin: 36-56 parts; low-viscosity phenolic-modified epoxy resin: 8-28 parts; benzyl glycidyl ether: 1-5 parts; calcium carbonate: 20-40 parts; white colorant: 0.5-4 parts; fumed silica: 0.05-0.4 part;
step (B), sequentially adding the modified epoxy resin, the low-viscosity phenolic aldehyde modified epoxy resin, the benzyl glycidyl ether, the calcium carbonate, the white colorant and the gas-phase silica in the step (A) into a stirring cylinder, dispersing and stirring for 30-50min, grinding by a grinding machine until the fineness is less than 80 mu m, defoaming, filtering and packaging to obtain a component A;
step (C), preparation of the component B, and preparation of the following components in parts by weight: polythiol: 50-70 parts; accelerator (b): 2-8 parts; epoxy reactive diluent: 0.5-4 parts; calcium carbonate: 20-35 parts; red colorant: 0.1-0.8 part; fumed silica: 0.02-0.3 part;
and (D) sequentially adding the polythiol, the accelerator, the epoxy active diluent, the calcium carbonate, the red colorant and the fumed silica in the step (C) into a stirring cylinder, dispersing and stirring for 35-55min, grinding by using a grinding machine until the fineness is less than 55 mu m, defoaming, filtering and packaging to obtain a component B.
The following description will be given to specific examples of the adhesive for solar grade silicon wafer suitable for large-size flaking and the preparation process and the using method thereof,
in example 1, a raw material of an adhesive for a solar-grade silicon wafer suitable for large-size flaking comprises the following components in parts by weight: wherein the component A comprises the following components in parts by weight: modified epoxy resin: 46 parts of (a); low-viscosity phenolic-modified epoxy resin: 18 parts of a mixture; benzyl glycidyl ether: 3 parts of a mixture; calcium carbonate: 30.8 parts; white colorant: 2 parts of (1); fumed silica: 0.2 part; the component B comprises the following components in parts by weight: polythiol: 64 parts of a binder; accelerator (b): 5.8 parts; epoxy reactive diluent: 2.2 parts of; calcium carbonate: 27.5 parts; red colorant: 0.4 part; fumed silica: 0.1 part;
the preparation process of example 1 is as follows:
a preparation process of an adhesive for solar-grade silicon wafers applicable to large-size flaking comprises the following steps,
step (A1), preparing the component A, wherein the component A comprises the following components in parts by weight: modified epoxy resin: 46 parts of (a); low-viscosity phenolic-modified epoxy resin: 18 parts of a mixture; benzyl glycidyl ether: 3 parts of a mixture; calcium carbonate: 30.8 parts; white colorant: 2 parts of (1); fumed silica: 0.2 part;
step (B1), sequentially adding the modified epoxy resin, the low-viscosity phenolic aldehyde modified epoxy resin, the benzyl glycidyl ether, the calcium carbonate, the white colorant and the gas-phase silicon dioxide in the step (A1) into a stirring cylinder, dispersing and stirring for 40min, grinding by a grinding machine until the fineness is less than 80 mu m, defoaming, filtering and packaging to obtain a component A;
step (C1), preparing the component B, preparing the following components in parts by weight: polythiol: 64 parts of a binder; accelerator (b): 5.8 parts; epoxy reactive diluent: 2.2 parts of; calcium carbonate: 27.5 parts; red colorant: 0.4 part; fumed silica: 0.1 part;
and (D1) adding the polythiol, the accelerator, the epoxy active diluent, the calcium carbonate, the red colorant and the fumed silica in the step (C1) into a stirring cylinder in sequence, dispersing and stirring for 45min, grinding by a grinding machine until the fineness is less than 55 mu m, defoaming, filtering and packaging to obtain a component B.
Embodiment 2, a raw material of a tacky adhesive for a large-size flaked solar-grade silicon wafer comprises the following components in parts by weight: wherein the component A comprises the following components in parts by weight: modified epoxy resin: 37 parts of; low-viscosity phenolic-modified epoxy resin: 10 parts of (A); benzyl glycidyl ether: 2 parts of (1); calcium carbonate: 30.8 parts; white colorant: 2 parts of a mixture; fumed silica: 0.2 part; the component B comprises the following components in parts by weight: polythiol: 50 parts of a binder; accelerator (b): 2 parts of a mixture; epoxy reactive diluent: 0.6 part; calcium carbonate: 27.5 parts; red colorant: 0.4 part; fumed silica: 0.1 part;
the preparation process of example 2 is as follows:
a preparation process of an adhesive for a large-size flaky solar-grade silicon wafer comprises the following steps,
step (A2), preparing the component A, wherein the component A comprises the following components in parts by weight: modified epoxy resin: 37 parts of; low-viscosity phenolic-modified epoxy resin: 10 parts of (A); benzyl glycidyl ether: 2 parts of a mixture; calcium carbonate: 30.8 parts; white colorant: 2 parts of (1); fumed silica: 0.2 part;
step (B2), sequentially adding the modified epoxy resin, the low-viscosity phenolic aldehyde modified epoxy resin, the benzyl glycidyl ether, the calcium carbonate, the white colorant and the gas-phase silica in the step (A2) into a stirring cylinder, dispersing and stirring for 40min, grinding by a grinding machine until the fineness is less than 80 mu m, and finally defoaming, filtering and packaging to obtain a component A;
step (C2), preparing the component B, wherein the following components are prepared and the weight parts of the components are as follows: polythiol: 50 parts of a mixture; accelerator (b): 2 parts of (1); epoxy reactive diluent: 0.6 part; calcium carbonate: 27.5 parts; red colorant: 0.4 part; fumed silica: 0.1 part;
and (D2) adding the polythiol, the accelerator, the epoxy active diluent, the calcium carbonate, the red colorant and the fumed silica in the step (C2) into a stirring cylinder in sequence, dispersing and stirring for 45min, grinding by a grinding machine until the fineness is less than 55 mu m, defoaming, filtering and packaging to obtain a component B.
Example 3, a raw material of an adhesive for a solar-grade silicon wafer suitable for large-size flaking includes the following components in parts by weight: wherein the component A comprises the following components in parts by weight: modified epoxy resin: 54 parts of a binder; low-viscosity phenolic-modified epoxy resin: 24 parts of (1); benzyl glycidyl ether: 4 parts of a mixture; calcium carbonate: 30.8 parts; white colorant: 2 parts of (1); fumed silica: 0.2 part; the component B comprises the following components in parts by weight: polythiol: 68 parts of (b); accelerator (b): 7 parts; epoxy reactive diluent: 3.5 parts; calcium carbonate: 27.5 parts; red colorant: 0.4 part; fumed silica: 0.1 part.
The preparation process of example 3 is as follows:
a preparation process of an adhesive for a large-size flaky solar-grade silicon wafer comprises the following steps,
step (A3), preparing the component A, preparing the following components in parts by weight: modified epoxy resin: 54 parts of a binder; low-viscosity phenolic-modified epoxy resin: 24 parts of (1); benzyl glycidyl ether: 4 parts; calcium carbonate: 30.8 parts; white colorant: 2 parts of (1); fumed silica: 0.2 part;
step (B3), sequentially adding the modified epoxy resin, the low-viscosity phenolic aldehyde modified epoxy resin, the benzyl glycidyl ether, the calcium carbonate, the white colorant and the gas-phase silica in the step (A3) into a stirring cylinder, dispersing and stirring for 40min, grinding by a grinding machine until the fineness is less than 80 mu m, and finally defoaming, filtering and packaging to obtain a component A;
step (C3), preparing the component B, preparing the following components in parts by weight: polythiol: 68 parts of (b); accelerator (b): 7 parts; epoxy reactive diluent: 3.5 parts; calcium carbonate: 27.5 parts; red colorant: 0.4 part; fumed silica: 0.1 part;
and (D3) sequentially adding the polythiol, the accelerator, the epoxy active diluent, the calcium carbonate, the red colorant and the fumed silica in the step (C3) into a stirring tank, dispersing and stirring for 45min, grinding by using a grinding machine until the fineness is less than 55 mu m, defoaming, filtering and packaging to obtain a component B.
The preparation process of the adhesive for the solar-grade silicon wafer suitable for large-size flaking is characterized in that the dispersing and stirring time in the step (C) is 40min, and the dispersing and stirring time in the step (D) is 45 min.
A method for using a viscose for a large-size flaky solar-grade silicon wafer is characterized in that a component A and a component B are uniformly mixed according to a mass ratio of 1: 1-1.2 for use.
According to the application method of the viscose for the solar-grade silicon wafer suitable for large-size flaking, the component A and the component B are uniformly mixed according to the mass ratio of 1: 1 for use.
Comparative example 1, a raw material of a tacky adhesive for a large-sized flaked solar-grade silicon wafer comprises the following components in parts by weight: wherein the component A comprises the following components in parts by weight: 66 parts of E51 epoxy resin, 31.8 parts of calcium carbonate, 2 parts of white colorant and 0.2 part of fumed silica; the component B comprises the following components in parts by weight: 66 parts of polythiol, 3 parts of accelerator, 30.4 parts of calcium carbonate, 0.5 part of blue colorant and 0.1 part of fumed silica;
the preparation process of comparative example 1 is as follows:
a preparation process of an adhesive for solar-grade silicon wafers applicable to large-size flaking comprises the following steps,
step (A4), preparing the component A, preparing the following components in parts by weight: 66 parts of E51 epoxy resin, 31.8 parts of calcium carbonate, 2 parts of white colorant and 0.2 part of fumed silica;
step (B4), sequentially adding the E51 epoxy resin, the calcium carbonate, the white colorant and the fumed silica in the step (A4) into a stirring cylinder, dispersing and stirring for 40min, grinding by a grinder until the fineness is less than 80 μm, defoaming, filtering and packaging to obtain a component A;
step (C4), preparing the component B, preparing the following components in parts by weight: 66 parts of polythiol, 3 parts of accelerator, 30.4 parts of calcium carbonate, 0.5 part of blue colorant and 0.1 part of fumed silica;
and (D4) sequentially adding the polythiol, the accelerator, the calcium carbonate, the blue colorant and the fumed silica in the step (C4) into a stirring cylinder, dispersing and stirring for 40min, grinding by using a grinding machine until the fineness is less than 60 mu m, defoaming, filtering and packaging to obtain a component B.
According to the viscose for the solar-grade silicon wafer suitable for large-size flaking and the preparation process and the using method thereof, data analysis is carried out as follows in the following tables 1 and 2:
Figure BDA0003701118380000151
Figure BDA0003701118380000161
table 1
Table 1 shows: the technical performance tables for the viscose adhesives of example 1 according to the invention and comparative example 1 are given below, where: blank no data, TG indicates: the adhesive is an adhesive film after being cured, wherein the higher the TG is, the higher the temperature resistance of the adhesive is, the better the adhesive is.
Figure BDA0003701118380000162
Figure BDA0003701118380000171
Table 2
Table 2 shows: the viscose adhesives in the embodiment 1 and the comparative example 1 are used for bonding 210mm, 182mm and 162-140 μm thick silicon rods, and are cured for more than 2 hours under the same process conditions to perform wire cutting, and the data table of the wire cutting is shown.
According to the invention, the modified epoxy resin and the low-viscosity phenolic aldehyde modified epoxy resin are used, so that the hardness of the adhesive film is increased, the TG of the adhesive film is improved, the heat resistance of the adhesive film is improved, the temperature rise of the adhesive film caused by the failure of heat to be taken away in time is resisted, the deformation of the adhesive film is reduced, the phenomena of sheet falling and high collapse rate of the adhesive surface of a silicon wafer caused by the reduction of the performance due to the damage of the adhesive film are avoided, the sheet falling rate and the collapse rate are reduced, and the qualified rate is improved; according to the invention, the viscosity of the adhesive is adjusted by adding benzyl glycidyl ether, the viscosity of the adhesive is reduced to be proper, the fluidity is improved, the thickness of the adhesive layer is controlled when a silicon rod is bonded, the problem of line hanging is solved, and the line hanging rate of the adhesive layer is reduced.
In summary, the present invention provides a viscose for a solar grade silicon wafer suitable for large-size flaking, and a preparation process and a use method thereof, and the following conclusions are drawn:
(1) as can be seen from table 1, the viscosity of the a component is 18600mpa.s and the viscosity of the B component is 20500mpa.s in example 1 of the adhesive of the present invention, and the viscosity of the a component is 42000mpa.s and the viscosity of the B component is 40000mpa.s in comparative example 1 of the adhesive of the prior art, and thus it is understood that the viscosity of the adhesive of the present invention is significantly reduced compared to the prior art, and the fluidity is significantly improved.
(2) As can be seen from table 2, in the silicon rod with the width of 210mm in the embodiment 1 of the viscose of the present invention and the comparative example 1 of the viscose of the prior art, the silicon rod is cured for more than 2 hours under the same process conditions for wire cutting, and when the number of the wire cutters is 800, the collapse rate of the viscose of the present invention is 1.85%, the line hanging rate of the glue layer is 0.1%, the collapse rate of the viscose of the prior art is 5.6%, and the line hanging rate of the glue layer is 10.8%, so that when the viscose of the present invention is used for bonding the silicon rod with the width of 210mm, the collapse rate is obviously reduced, the yield is improved, and the line hanging rate of the glue layer is obviously reduced;
as can be seen from table 2, in the silicon rod with a width of 182mm in the embodiment 1 of the viscose of the present invention and the comparative example 1 of the viscose of the prior art, when the silicon rod is cured for more than 2 hours under the same process conditions for wire cutting, and the number of wire cutting knives is 1500, the collapse rate of the viscose of the present invention is 1.6%, the wire hanging rate of the glue layer is 0.05%, the collapse rate of the viscose of the prior art is 4.8%, and the wire hanging rate of the glue layer is 8.5%, so that when the viscose of the present invention is used for bonding the silicon rod with a width of 182mm, the collapse rate is significantly reduced, the yield is improved, and the wire hanging rate of the glue layer is significantly reduced;
as can be seen from table 2, in the silicon rod with the width dimension of 162 μm and the thickness of 140 μm in the adhesive example 1 of the invention and the adhesive comparative example 1 of the prior art, the silicon rod is cured for more than 2 hours under the same process conditions for wire cutting, and when the number of wire cutters is 800, the collapse rate of the adhesive of the invention is 1.45%, the sheet drop rate is 0.001%, and the collapse rate of the adhesive of the prior art is 2.9%, and the sheet drop rate is 1.3%.
(3) As can be seen from tables 1 and 2, when compared with the prior art, the viscose of the invention is used for cutting large sizes of 182mm and 210mm by using diamond wires with wire diameters of 38 μm and 40 μm, the chipping rate can be effectively reduced, and is reduced from 5.6% to below 1.5%; cutting 162-140 μm thick sheet with 38 μm and 40 μm diamond wire, and reducing collapse rate to below 1.5%; the sheet dropping rate can be reduced from 1.3% to 0% due to the improvement of the heat resistance of the adhesive layer; because the viscosity is low and the fluidity is excellent, the thickness of the adhesive layer can be effectively controlled to be 0.16-0.2mm when the adhesive stick is adhered, and the thread hanging rate of the adhesive layer is reduced from 10.8% to 0.1%.
By using the viscose of the invention, the enterprise benefits can be increased as follows: the wafer breakage rate is reduced from 5.6% to 1.5% according to 200 ten thousand silicon wafers, the wafer B is reduced by 200 x 4.1% to 8.2 ten thousand wafers, the price difference between the wafer A and the wafer B is 1.29 yuan in 2022, an enterprise can generate 8.2 x 1.29 yuan to 10.57 ten thousand yuan per 200 ten thousand wafers, the wafer breakage rate is reduced from 1.3% to 0%, the wafer A is reduced by 200.3% to 2.6 ten thousand wafers, each wafer is 6.45 yuan, the yield generated by the enterprise per 200 ten thousand wafers is 6.45 x 2.6 yuan to 16.77 ten thousand wafers, wherein the wafer A is a qualified product, and the wafer B is a degraded inferior product.
The foregoing illustrates and describes the principles, general features, and advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are given by way of illustration of the principles of the present invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, and such changes and modifications are within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (8)

1. The adhesive for the solar-grade silicon wafer suitable for large-size flaking is characterized by comprising a component A and a component B;
the component A comprises the following components in parts by weight:
modified epoxy resin: 36-56 parts;
low-viscosity phenolic-modified epoxy resin: 8-28 parts;
benzyl glycidyl ether: 1-5 parts;
calcium carbonate: 20-40 parts;
white colorant: 0.5-4 parts;
fumed silica: 0.05-0.4 part;
the component B comprises the following components in parts by weight:
polythiol: 50-70 parts;
accelerator (b): 2-8 parts;
epoxy reactive diluent: 0.5-4 parts;
calcium carbonate: 20-35 parts;
red colorant: 0.1-0.8 part;
fumed silica: 0.02-0.3 part.
2. The adhesive for solar-grade silicon wafers suitable for large-size flaking according to claim 1, characterized by comprising a component A and a component B;
the component A comprises the following components in parts by weight:
modified epoxy resin: 46 parts of (a);
low-viscosity phenolic-modified epoxy resin: 18 parts of a mixture;
benzyl glycidyl ether: 3 parts of a mixture;
calcium carbonate: 30.8 parts;
white colorant: 2 parts of (1);
fumed silica: 0.2 part;
the component B comprises the following components in parts by weight:
polythiol: 64 parts;
accelerator (b): 5.8 parts;
epoxy reactive diluent: 2.2 parts of;
calcium carbonate: 27.5 parts;
red colorant: 0.4 part;
fumed silica: 0.1 part.
3. The adhesive for solar-grade silicon wafers suitable for large-size flaking according to claim 1, characterized by comprising a component A and a component B;
the component A comprises the following components in parts by weight:
modified epoxy resin: 37 parts of;
low-viscosity phenolic-modified epoxy resin: 10 parts of a binder;
benzyl glycidyl ether: 2 parts of (1);
calcium carbonate: 30.8 parts;
white colorant: 2 parts of (1);
fumed silica: 0.2 part;
the component B comprises the following components in parts by weight:
polythiol: 50 parts of a mixture;
accelerator (b): 2 parts of a mixture;
epoxy reactive diluent: 0.6 part;
calcium carbonate: 27.5 parts;
red colorant: 0.4 part;
fumed silica: 0.1 part.
4. The adhesive for solar-grade silicon wafers suitable for large-size flaking according to claim 1, characterized by comprising a component A and a component B;
the component A comprises the following components in parts by weight:
modified epoxy resin: 54 parts of a binder;
low-viscosity phenolic-modified epoxy resin: 24 parts of (1);
benzyl glycidyl ether: 4 parts of a mixture;
calcium carbonate: 30.8 parts;
white colorant: 2 parts of (1);
fumed silica: 0.2 part;
the component B comprises the following components in parts by weight:
polythiol: 68 parts of (b);
accelerator (b): 7 parts;
epoxy reactive diluent: 3.5 parts;
calcium carbonate: 27.5 parts;
red colorant: 0.4 part;
fumed silica: 0.1 part.
5. A preparation process of an adhesive for a solar-grade silicon wafer suitable for large-size flaking is characterized by comprising the following steps,
step (A), preparing the component A, namely preparing the following components in parts by weight: modified epoxy resin: 36-56 parts; low-viscosity phenolic-modified epoxy resin: 8-28 parts; benzyl glycidyl ether: 1-5 parts; calcium carbonate: 20-40 parts; white colorant: 0.5-4 parts; fumed silica: 0.05-0.4 part;
step (B), sequentially adding the modified epoxy resin, the low-viscosity phenolic aldehyde modified epoxy resin, the benzyl glycidyl ether, the calcium carbonate, the white colorant and the gas-phase silica in the step (A) into a stirring cylinder, dispersing and stirring for 30-50min, grinding by a grinding machine until the fineness is less than 80 mu m, defoaming, filtering and packaging to obtain a component A;
step (C), preparing the component B, namely preparing the following components in parts by weight: polythiol: 50-70 parts; accelerator (b): 2-8 parts; epoxy reactive diluent: 0.5-4 parts; calcium carbonate: 20-35 parts; red colorant: 0.1-0.8 part; fumed silica: 0.02-0.3 part;
and (D) sequentially adding the polythiol, the accelerator, the epoxy active diluent, the calcium carbonate, the red colorant and the fumed silica in the step (C) into a stirring cylinder, dispersing and stirring for 35-55min, grinding by using a grinding machine until the fineness is less than 55 mu m, defoaming, filtering and packaging to obtain a component B.
6. The process for preparing the adhesive for the solar-grade silicon wafer applicable to the large-size flaking according to claim 5, characterized in that the dispersion stirring time in step (C) is 40min and the dispersion stirring time in step (D) is 45 min.
7. The application method of the adhesive for the solar-grade silicon wafer suitable for large-size flaking is characterized in that the component A and the component B are uniformly mixed according to the mass ratio of 1: 1-1.2 for use.
8. The use method of the viscose glue for the solar-grade silicon wafer suitable for large-size flaking as claimed in claim 7, characterized in that the component A and the component B are uniformly mixed according to the mass ratio of 1: 1.
CN202210693142.5A 2022-06-17 2022-06-17 Adhesive for solar-grade silicon wafer suitable for large-size flaking and preparation process and use method thereof Pending CN114921210A (en)

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Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5166228A (en) * 1990-08-14 1992-11-24 Shin-Etsu Chemical Co., Ltd. Epoxy resin compositions containing polysubstituted novolac epoxy resins and naphthylene based phenolic resin curing agents and semiconductor devices encapsulated therewith
CN103497722A (en) * 2013-10-10 2014-01-08 南宁珀源化工有限公司 Adhesive for adhering silicon rods
CN103571411A (en) * 2013-01-16 2014-02-12 上海都为电子有限公司 Dual-component epoxy resin adhesive for splicing silicon block or silicon rod and preparation method of dual-component epoxy resin adhesive
CN106634760A (en) * 2016-12-29 2017-05-10 安徽浩丰特种电子材料有限公司 Epoxy resin pouring sealant with excellent mechanical properties
CN106883803A (en) * 2017-03-09 2017-06-23 苏州润德新材料有限公司 A kind of single-component adhesive of silicon rod fixation
CN112646524A (en) * 2020-12-23 2021-04-13 重庆德天汽车新材料研究院有限公司 Single-component epoxy adhesive for bonding self-lubricating steel plates and preparation method thereof
CN112852367A (en) * 2021-03-08 2021-05-28 南宁珀源能源材料有限公司 Double-component silicon rod splicing adhesive and preparation method thereof
CN113913139A (en) * 2021-09-18 2022-01-11 惠州市杜科新材料有限公司 Waterproof high-temperature-resistant single-component epoxy sealing adhesive for Type-c connector and preparation method thereof
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
CN114539960A (en) * 2021-12-03 2022-05-27 苏州乐文高分子材料科技有限公司 Bi-component epoxy resin adhesive and preparation method thereof

Patent Citations (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5166228A (en) * 1990-08-14 1992-11-24 Shin-Etsu Chemical Co., Ltd. Epoxy resin compositions containing polysubstituted novolac epoxy resins and naphthylene based phenolic resin curing agents and semiconductor devices encapsulated therewith
CN103571411A (en) * 2013-01-16 2014-02-12 上海都为电子有限公司 Dual-component epoxy resin adhesive for splicing silicon block or silicon rod and preparation method of dual-component epoxy resin adhesive
CN103497722A (en) * 2013-10-10 2014-01-08 南宁珀源化工有限公司 Adhesive for adhering silicon rods
CN106634760A (en) * 2016-12-29 2017-05-10 安徽浩丰特种电子材料有限公司 Epoxy resin pouring sealant with excellent mechanical properties
CN106883803A (en) * 2017-03-09 2017-06-23 苏州润德新材料有限公司 A kind of single-component adhesive of silicon rod fixation
CN112646524A (en) * 2020-12-23 2021-04-13 重庆德天汽车新材料研究院有限公司 Single-component epoxy adhesive for bonding self-lubricating steel plates and preparation method thereof
CN112852367A (en) * 2021-03-08 2021-05-28 南宁珀源能源材料有限公司 Double-component silicon rod splicing adhesive and preparation method thereof
CN113913139A (en) * 2021-09-18 2022-01-11 惠州市杜科新材料有限公司 Waterproof high-temperature-resistant single-component epoxy sealing adhesive for Type-c connector and preparation method thereof
CN114539960A (en) * 2021-12-03 2022-05-27 苏州乐文高分子材料科技有限公司 Bi-component epoxy resin adhesive and preparation method thereof
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

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
高学敏等: "《粘接和粘接技术手册》", vol. 1, 四川科学技术出版社, pages: 395 *

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