CN115651580B - Epoxy resin adhesive and preparation method and application thereof - Google Patents
Epoxy resin adhesive and preparation method and application thereof Download PDFInfo
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- CN115651580B CN115651580B CN202211393973.7A CN202211393973A CN115651580B CN 115651580 B CN115651580 B CN 115651580B CN 202211393973 A CN202211393973 A CN 202211393973A CN 115651580 B CN115651580 B CN 115651580B
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 65
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 65
- 239000000853 adhesive Substances 0.000 title claims abstract description 47
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 110
- 239000000945 filler Substances 0.000 claims abstract description 79
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229910021421 monocrystalline silicon Inorganic materials 0.000 claims abstract description 55
- 239000011863 silicon-based powder Substances 0.000 claims abstract description 47
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 44
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 23
- 239000010703 silicon Substances 0.000 claims abstract description 23
- 239000003292 glue Substances 0.000 claims abstract description 20
- 229920006295 polythiol Polymers 0.000 claims abstract description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 46
- 239000004408 titanium dioxide Substances 0.000 claims description 22
- 229910021485 fumed silica Inorganic materials 0.000 claims description 19
- 239000007822 coupling agent Substances 0.000 claims description 15
- 239000003085 diluting agent Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000000034 method Methods 0.000 claims description 4
- 229910002012 Aerosil® Inorganic materials 0.000 claims description 3
- 235000010215 titanium dioxide Nutrition 0.000 claims 4
- 229920006335 epoxy glue Polymers 0.000 claims 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 28
- 238000005520 cutting process Methods 0.000 abstract description 26
- 239000002245 particle Substances 0.000 abstract description 23
- 239000002210 silicon-based material Substances 0.000 abstract description 5
- 239000002699 waste material Substances 0.000 abstract description 5
- 210000001503 joint Anatomy 0.000 abstract description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 22
- 239000000843 powder Substances 0.000 description 17
- 229910000019 calcium carbonate Inorganic materials 0.000 description 11
- 239000000084 colloidal system Substances 0.000 description 10
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 description 9
- 239000002002 slurry Substances 0.000 description 9
- 239000011256 inorganic filler Substances 0.000 description 7
- 229910003475 inorganic filler Inorganic materials 0.000 description 7
- 239000000243 solution Substances 0.000 description 7
- 238000003756 stirring Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 4
- CDQSJQSWAWPGKG-UHFFFAOYSA-N butane-1,1-diol Chemical compound CCCC(O)O CDQSJQSWAWPGKG-UHFFFAOYSA-N 0.000 description 4
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 239000003921 oil Substances 0.000 description 4
- 229910021487 silica fume Inorganic materials 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000004593 Epoxy Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 2
- 239000012790 adhesive layer Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000002715 modification method Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- MXRIRQGCELJRSN-UHFFFAOYSA-N O.O.O.[Al] Chemical compound O.O.O.[Al] MXRIRQGCELJRSN-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000001038 titanium pigment Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention relates to the field of adhesives, and provides an epoxy resin adhesive and a preparation method and application thereof, wherein the epoxy resin adhesive comprises an A component and a B component, the A component comprises epoxy resin and a first filler, the first filler comprises silicon dioxide and monocrystalline silicon powder with different particle diameters, and the mass fraction of the first filler in the A component is 75-85%; the component B comprises polythiol and a second filler, the second filler comprises monocrystalline silicon powder with different particle sizes, and the mass fraction of the second filler in the component B is 55-70%. The Mohs hardness of the cured epoxy resin adhesive reaches 6, and the density is 2.1-2.3g/cm 3 The hardness and density of the single crystal silicon rod are close to those of the single crystal silicon rod, and the glue is used for filling the butt joint of the silicon rod and the inclined planes at the two ends, so that the glue can directly participate in cutting, a wire division net is not needed, the silicon material waste can be effectively reduced, and the cutting efficiency is improved.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to an epoxy resin adhesive and a preparation method and application thereof.
Background
In the photovoltaic slicing industry, the silicon rods are provided with inclined planes at two ends before being cut, and the multi-splicing rods are provided with splicing seams for splicing the silicon rods. The wire diameter of the steel wire is gradually reduced, the wire is easier to break, and in order to prevent the wire breakage caused by the inclined planes and the edge joints during cutting, the inclined planes and the edge joints at the two ends of the silicon rod are required to be separated by a wire separation net technology, so that the cutting is not participated. The inclined planes at the two ends of the single rod need to be removed, each end is about 2mm, 4 sheets can be produced per mm, each cutter wastes 4mm, and about 16 sheets are produced less; the double-spliced rod needs to remove 8mm and 32 pieces are fewer; the three-piece stick needs to be removed by 12mm and 48 pieces are fewer. Silicon material waste is serious at two ends of the silicon rod and the splicing seam.
The existing epoxy resin rod splicing glue in the slicing industry can only provide bonding strength, plays a role in splicing silicon rods, and does not participate in cutting. The Mohs hardness of the existing bar glue is 3, and the density is 1.4-1.5g/cm 3 The conductivity is 50-200us/cm, the Mohs hardness of the single crystal silicon rod is 7, and the density is 2.33g/cm 3 The conductivity of the slurry system for cutting the silicon wafer is 25-30us/cm. If the existing rod splicing glue participates in cutting, the problems of high and low lines, jumper wires and the like caused by overlarge difference of two media in the cutting process cannot be solved because the hardness and the density are far lower than those of a silicon rod, so that broken lines cannot be controlled.
Disclosure of Invention
The invention provides an epoxy resin adhesive, a preparation method and application thereof, which are used for solving the defects of silicon material waste and low cutting efficiency in the prior art, so that the epoxy resin adhesive can be used for bonding silicon rods and can be directly used for cutting.
The invention provides an epoxy resin adhesive, which comprises an A component and a B component, wherein the A component comprises epoxy resin and a first filler, the first filler comprises silicon dioxide and monocrystalline silicon powder with different particle diameters, and the mass fraction of the first filler in the A component is 75-85%;
the component B comprises polythiol and a second filler, the second filler comprises monocrystalline silicon powder with different particle sizes, and the mass fraction of the second filler in the component B is 55-70%.
According to the epoxy resin adhesive provided by the invention, the first filler comprises, by weight, 7-9 parts of silica micropowder with a D50 of 10um, 7-9 parts of silica micropowder with a D50 of 6um, 33-37 parts of silica micropowder with a D50 of 4um, 9-11 parts of silica micropowder with a D50 of 2.5um and 4-6 parts of monocrystalline silicon powder with a D50 of 1 um.
According to the epoxy resin adhesive provided by the invention, the first filler also comprises titanium dioxide, and the mass ratio of silicon dioxide, monocrystalline silicon powder and titanium dioxide in the first filler is 60-65:5-10:10-20.
The epoxy resin adhesive provided by the invention further comprises a reactive diluent and fumed silica, wherein the A component comprises the following components in percentage by mass: 11-20% of epoxy resin, 75-85% of first filler, 3.5-5% of reactive diluent and 0.1-0.3% of fumed silica.
According to the epoxy resin adhesive provided by the invention, the second filler comprises, by weight, 14-16 parts of monocrystalline silicon powder with the D50 of 4um, 18-22 parts of monocrystalline silicon powder with the D50 of 2um and 18-22 parts of monocrystalline silicon powder with the D50 of 500 nm.
According to the epoxy resin adhesive provided by the invention, the second filler also comprises titanium dioxide, and in the second filler, the mass ratio of the monocrystalline silicon powder to the titanium dioxide is 50-60:10-20.
The epoxy resin adhesive provided by the invention further comprises an accelerator and fumed silica, wherein the component B comprises the following components in percentage by mass: 20-35% of polythiol, 55-70% of second filler, 7-10% of accelerator and 0.1-0.3% of aerosil.
According to the epoxy resin adhesive provided by the invention, the first filler and the second filler are subjected to surface modification by using the coupling agent, wherein the coupling agent is selected from titanate coupling agents accounting for 0.5-1% of the filler and silane coupling agents accounting for 2-5% of the filler.
The invention also provides a preparation method of the epoxy resin adhesive, which comprises the following steps: and respectively mixing and dispersing the raw materials of the component A and the component B, and then mixing the component A and the component B.
The invention also provides application of the epoxy resin adhesive in bonding silicon rods.
The invention provides an epoxy resin adhesive and a preparation method and application thereof. The Mohs hardness of the cured epoxy resin adhesive reaches 6, and the density is 2.1-2.3g/cm 3 The hardness and density of the single crystal silicon rod are close to those of the single crystal silicon rod, and the glue is used for filling the butt joint of the silicon rod and the inclined planes at the two ends, so that the glue can directly participate in cutting, a wire division net is not needed, the silicon material waste can be effectively reduced, and the cutting efficiency is improved.
Furthermore, the conductivity of the epoxy resin adhesive is lower than 20us/cm, the pH is 7-8, and the properties of the adhesive powder produced by cutting in various aspects such as the conductivity of the slurry system can not be influenced basically when the adhesive powder enters the slurry system.
Drawings
In order to more clearly illustrate the invention or the technical solutions of the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described, and it is obvious that the drawings in the description below are some embodiments of the invention, and other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 is a schematic diagram of the epoxy resin adhesive in example 1 of the present invention after bonding the silicon rod.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In a first aspect, the invention provides an epoxy resin adhesive, which comprises an A component and a B component, wherein the A component comprises epoxy resin and a first filler, the first filler comprises silicon dioxide and monocrystalline silicon powder with different particle diameters, and the mass fraction of the first filler in the A component is 75-85%;
the component B comprises polythiol and a second filler, the second filler comprises monocrystalline silicon powder with different particle sizes, and the mass fraction of the second filler in the component B is 55-70%.
In the prior art, the epoxy resin rod splicing glue can only provide bonding strength, plays a role in splicing silicon rods, and does not participate in cutting. The invention researches find that the epoxy resin adhesive used for the splicing seam of the silicon rod and the filling of the two ends and capable of being directly cut can be improved from the filling. The filler in the epoxy resin glue is usually one or more of silicon micropowder, alumina powder, magnesia powder, titanium pigment, aluminum hydroxide powder and calcium carbonate, more commonly calcium carbonate and aluminum hydroxide. According to the invention, silicon dioxide and monocrystalline silicon powder with different particle sizes are adopted in the component A, monocrystalline silicon powder with different particle sizes is adopted in the component B, and the filling material ratio is controlled within the range, so that the glue with hardness and density close to those of monocrystalline silicon can be obtained on the premise of not influencing the performance of the epoxy resin glue, and the epoxy resin glue can be directly cut after bonding the two ends of a silicon rod or filling the silicon rod, so that the silicon material is saved, and the cutting efficiency is also improved.
The epoxy resin of the present invention is bisphenol a type epoxy resin, for example, E51 epoxy resin.
In some embodiments of the invention, the first filler comprises, in parts by weight, 7-9 parts of a silica fume having a D50 of 10um, 7-9 parts of a silica fume having a D50 of 6um, 33-37 parts of a silica fume having a D50 of 4um, 9-11 parts of a silica fume having a D50 of 2.5um, and 4-6 parts of a monocrystalline silicon powder having a D50 of 1 um.
In order to further improve the hardness, the compactness of the adhesive layer is higher, when the silica and the monocrystalline silicon powder filler are added, the micro powder with different particle sizes is used for grading matching, gaps among the micro powder are made up, the adhesive layer has higher compactness, and the hardness after solidification is close to that of a monocrystalline silicon rod. In addition, the filler such as silicon dioxide with large particle size, monocrystalline silicon powder and the like has smaller specific surface area and lower oil absorption value, is easier to wet, and is beneficial to reducing the proportion of liquid materials. However, if the component A is doped with the silica micro powder with the particle D50 larger than 10um, micro air holes are easy to appear on the surface glue layer after the glue is solidified, and the possibility of broken lines in the cutting process exists, so that the particle size of the silica micro powder D50 is maximally selected to be 10 um.
In some embodiments of the invention, the first filler further comprises titanium dioxide, and the mass ratio of the silicon dioxide, the monocrystalline silicon powder and the titanium dioxide in the first filler is 60-65:5-10:10-20.
The edge joint participates in cutting, the cutting depth of the existing silicon rod is generally 188-218, a large amount of rubber powder in the cutting process can enter a slurry system, and if the existing epoxy resin adhesive is still adopted, the conductivity of the slurry system can not be controlled. According to the invention, a certain proportion of titanium dioxide is added into the first filler, so that the pH and conductivity can be reduced, and the colloid density can be improved.
In some embodiments of the present invention, the a-component further comprises a reactive diluent and fumed silica, the a-component comprising, in mass percent: 11-20% of epoxy resin, 75-85% of first filler, 3.5-5% of reactive diluent and 0.1-0.3% of fumed silica.
In the above technical solution, the reactive diluent is added to reduce the viscosity of the colloid, and the reactive diluent may be epoxy reactive diluent commonly used in the art, such as 1, 4-butanediol. The fumed silica is added to serve as an anti-settling agent, so that the stability of the component A can be effectively maintained, and settling in the storage process can be prevented. Under the above formula, the density of the component A is 2.2-2.3g/cm 3 Between them.
In some embodiments of the invention, the second filler comprises, in parts by weight, 14-16 parts of single crystal silicon powder having a D50 of 4um, 18-22 parts of single crystal silicon powder having a D50 of 2um, and 18-22 parts of single crystal silicon powder having a D50 of 500 nm.
The different particle sizes of the second filler in the component B are matched in a grading manner, and the different particle sizes in the component A cannot be completely matched in a grading manner, the silicon dioxide in the component A is divided into four particle size grades of 10um, 6um, 4um and 2.5um, the matching of the silicon dioxide in the component A with 1um of the monocrystalline silicon powder is proper, and the component B is only divided into three grades of 4um, 2um and 500nm through research.
In some embodiments of the invention, the second filler further comprises titanium dioxide, and in the second filler, the mass ratio of the monocrystalline silicon powder to the titanium dioxide is 50-60:10-20.
In the invention, a certain amount of titanium dioxide is also added into the second filler to assist in adjusting pH, density and conductivity.
In some embodiments of the invention, the B component further comprises a promoter and fumed silica, the B component comprising, in mass percent: 20-35% of polythiol, 55-70% of second filler, 7-10% of accelerator and 0.1-0.3% of aerosil.
In the above technical solution, the accelerator is added to accelerate the mixing and curing speed of A, B components, and the accelerator can be selected from accelerators commonly used in the field, such as 2,4, 6-tris (dimethylaminomethyl) phenol, abbreviated as DMP-30. The fumed silica is added to serve as an anti-settling agent, so that the stability of the component A can be effectively maintained, and settling in the storage process can be prevented. Under the above formula, the density of the obtained component B is 2.05-2.15g/cm 3 Between them. The density of the finally obtained epoxy resin adhesive is 2.1-2.3g/cm by matching with the better formula of the component A 3 Between which the mohs hardness reaches 6.
It will be appreciated that the epoxy resin glue of the present invention may also include other components and adjuvants as desired, such as colorants, in amounts determined by means of conventional techniques in the art, without interfering with the formulation of the present invention.
In some embodiments of the present invention, the first filler and the second filler are both surface modified with a coupling agent selected from the group consisting of titanate coupling agents in an amount of 0.5-1% of the filler and silane coupling agents in an amount of 2-5% of the filler.
In order to obtain the glue with low conductivity, pH value and high filling, the conductivity, pH value and oil absorption value of the inorganic filler are preferably further reduced before preparation, the used inorganic filler needs to be subjected to surface activation modification by using a coupling agent, the modified filler surface is wrapped by the coupling agent, ionization of ions is reduced, the coupling agent surface is an oleophobic group, the oil absorption value of the filler can be reduced, and the filler is easier to disperse uniformly.
In a preferred embodiment of the invention, the specific modification method is as follows: firstly, adding a certain mass of inorganic filler into a heatable high-speed mixer, setting the heating temperature to 120 ℃, and stirring at a low speed to fully dry the moisture of the inorganic filler. After the filler is dried, adding titanate coupling agent accounting for 0.5-1% of the total filler, adding silane coupling agent accounting for 2-5% of the total filler into a spray tank, stirring and dispersing in a closed state, uniformly spraying the coupling agent onto the surface of the filler in a spray state through compressed air, and activating for 1 hour at 120 ℃ to obtain the inorganic filler with low conductivity, low pH value (the conductivity is lower than 10us/cm, the pH value is 7-8) and low oil absorption value.
The invention also provides a preparation method of the epoxy resin adhesive, which comprises the following steps: and respectively mixing and dispersing the raw materials of the component A and the component B, and then mixing the component A and the component B.
Wherein, in the process of respectively mixing and dispersing the raw materials of the component A and the component B, a high-speed dispersing machine can be adopted for dispersing and mixing. Bubbles may be generated due to high-speed dispersion, and then moderate defoaming may be performed.
The mass ratio of the component A to the component B is 1:1.
The invention also provides application of the epoxy resin adhesive in bonding silicon rods. The epoxy resin adhesive can be used for splicing joints of silicon rods and filling two ends, and the silicon rods obtained after application can be directly cut at the bonding positions without adopting a wire-dividing network technology, so that the cutting efficiency is improved.
The following is a description of specific examples.
Example 1
The embodiment provides an epoxy resin adhesive, which comprises the following components:
and (3) a component A: 14.5% of E51 epoxy resin, 61% of silicon dioxide with different particle sizes, 5% of monocrystalline silicon powder, 15% of titanium dioxide, 4.3% of butanediol and 0.2% of fumed silica;
wherein, the silicon dioxide with different particle diameters is specifically silicon dioxide micropowder with D50 of 10um (model HY-G5), 8 percent of silicon dioxide micropowder with D50 of 6um (model HY-G7), 35 percent of silicon dioxide micropowder with D50 of 4um (model HY-G10), and 10 percent of silicon dioxide micropowder with D50 of 2.5um (model HY-G12);
the D50 of the monocrystalline silicon powder is 1um;
the titanium dioxide D50 is 400nm.
And the component B comprises the following components: 27.5% of polythiol, 55% of monocrystalline silicon powder with different particle sizes, 10% of titanium dioxide, 7.3% of DMP-30 (2, 4, 6-tris (dimethylaminomethyl) phenol) and 0.2% of fumed silica;
wherein, the monocrystalline silicon powder with different grain diameters is specifically 15 percent of monocrystalline silicon powder with D50 of 4um, 20 percent of monocrystalline silicon powder with D50 of 2um and 20 percent of monocrystalline silicon powder with D50 of 500 nm;
the titanium dioxide D50 is 400nm.
The densities of the raw materials and the colloid are shown in Table 1.
TABLE 1
The preparation of the epoxy resin adhesive is as follows:
and (3) preparation of the component A: 14.5 parts of E51 epoxy resin, 8 parts of silica micropowder (model HY-G5) with the D50 of 10um, 8 parts of silica micropowder (model HY-G7) with the D50 of 6um, 35 parts of silica micropowder (model HY-G10) with the D50 of 4um, 10 parts of silica micropowder (model HY-G12) with the D50 of 2.5um, 5 parts of monocrystalline silicon powder with the D50 of 1um, 15 parts of titanium dioxide, 0.2 part of fumed silica serving as an anti-settling agent and 4.3 parts of epoxy reactive diluent (1, 4-butanediol) are added into a reactor to reduce the colloid viscosity. Dispersing and stirring for 2 hours in a high-speed dispersing machine, and then starting a vacuum pump to defoam for 1 hour to prepare the component A.
And (3) preparation of a component B: 27.5 parts of polythiol, 15 parts of monocrystalline silicon powder with the D50 of 4um, 20 parts of monocrystalline silicon powder with the D50 of 2um, 20 parts of monocrystalline silicon powder with the D50 of 500nm, 10 parts of titanium dioxide, 7.3 parts of accelerator (DMP-30) and 0.2 part of fumed silica serving as an anti-settling agent are added into a reactor. Dispersing and stirring for 2 hours in a high-speed dispersing machine, and then starting a vacuum pump to defoam for 1 hour to prepare the component B.
And mixing the component A and the component B according to the mass ratio of 1:1 to obtain the epoxy resin adhesive. The epoxy resin adhesive of the embodiment is adopted to bond silicon rods, the obtained physical diagram is shown in figure 1, the Mohs hardness of the cured epoxy resin adhesive of the embodiment reaches 6, and the density is 2.1-2.3g/cm 3 The cutting can be directly performed, the conductivity of the colloid is lower than 20us/cm, the pH is 7-8, and the property of the colloid in various aspects such as the conductivity of the slurry system can not be basically influenced when the rubber powder generated by cutting enters the slurry system.
Example 2
The embodiment provides an epoxy resin adhesive, which comprises the following components:
and (3) a component A: 14.5% of E51 epoxy resin, 61% of silicon dioxide with different particle sizes, 5% of monocrystalline silicon powder, 15% of titanium dioxide, 4.3% of butanediol and 0.2% of fumed silica;
wherein, the silicon dioxide with different particle diameters is specifically 8 percent of silicon dioxide micropowder with D50 of 10um, 8 percent of silicon dioxide micropowder with D50 of 6um, 35 percent of silicon dioxide micropowder with D50 of 4um and 10 percent of silicon dioxide micropowder with D50 of 2.5 um;
the D50 of the monocrystalline silicon powder is 1um;
the titanium dioxide D50 is 400nm.
And the component B comprises the following components: 27.5% of polythiol, 55% of monocrystalline silicon powder with different particle sizes, 10% of titanium dioxide, 7.3% of DMP-30 (2, 4, 6-tris (dimethylaminomethyl) phenol) and 0.2% of fumed silica;
wherein, the monocrystalline silicon powder with different grain diameters is specifically 15 percent of monocrystalline silicon powder with D50 of 4um, 20 percent of monocrystalline silicon powder with D50 of 2um and 20 percent of monocrystalline silicon powder with D50 of 500 nm;
the titanium dioxide D50 is 400nm.
Moreover, the fillers in the component A and the component B are subjected to surface modification of the coupling agent in advance, and the specific modification method is as follows: firstly, adding a certain mass of inorganic filler into a heatable high-speed mixer, setting the heating temperature to 120 ℃, and stirring at a low speed to fully dry the moisture of the inorganic filler. After the filler is dried, adding titanate coupling agent accounting for 0.5 percent of the total filler, adding silane coupling agent (KH 560) accounting for 3 percent of the total filler into a spray tank, stirring and dispersing in a closed state, uniformly spraying the coupling agent on the surface of the filler in a spray state through compressed air, and activating for 1 hour at the temperature of 120 ℃ to obtain the improved filler.
The preparation method of the epoxy resin adhesive is the same as that of example 1.
As a result, the epoxy resin adhesive of the present example had a Mohs hardness of 6 and a density of 2.1 to 2.3g/cm after curing 3 The cutting can be directly performed, the conductivity of the colloid is lower than 10us/cm, the pH is 7-8, and the property of the colloid in various aspects such as the conductivity of the slurry system can not be basically influenced when the rubber powder generated by cutting enters the slurry system.
Comparative example 1
The comparative example provides an epoxy resin adhesive, which comprises the following components:
and (3) a component A: 14.5% of E51 epoxy resin, 61% of silicon dioxide with different particle diameters, 5% of tungsten carbide micro powder, 15% of calcium carbonate, 4.3% of butanediol and 0.2% of fumed silica;
wherein, the silicon dioxide with different particle diameters is specifically 8 percent of silicon dioxide micropowder with D50 of 10um, 8 percent of silicon dioxide micropowder with D50 of 6um, 35 percent of silicon dioxide micropowder with D50 of 4um and 10 percent of silicon dioxide micropowder with D50 of 2.5 um;
the D50 of the tungsten carbide micro powder is 1um;
the calcium carbonate D50 was 400nm.
And the component B comprises the following components: 78% of polythiol, 14% of calcium carbonate, 4% of DMP-30 (2, 4, 6-tris (dimethylaminomethyl) phenol), 0.5% of fumed silica and 3.5% of butanediol.
In the comparative example, the component B adopts a conventional epoxy resin glue filler formula, and the component A is added with ultra-high hardness tungsten carbide powder, so that the Mohs hardness of the glue after curing reaches 7, and the density is 2.375g/cm 3 The hardness and the density performance are basically consistent with those of the monocrystalline silicon rod, but in the cutting process, the diamond wire with the wire diameter of 35-40um cannot be cut through colloid, and the wire bow at the joint reaches 40mm and then is broken. Colloid millThe conductivity of the cut powder is 19us/cm, and the tungsten carbide, the calcium carbonate and the silicon dioxide in the glue are cancelled one by one to cancel the regrinding test, so that the reason for the conductivity increase is the calcium carbonate powder, and the possible reason for the conductivity increase is that although the calcium carbonate is insoluble in water: 1) The calcium carbonate produces a slight ionization in aqueous solution, producing OH - Ions; 2) The calcium carbonate powder is further ground and thinned in cutting, so that ionization phenomenon is more easily generated. Therefore, calcium carbonate is discarded as a filler in the present invention.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. The epoxy resin adhesive is characterized by comprising an A component and a B component, wherein the A component comprises epoxy resin and a first filler, and the mass fraction of the first filler in the A component is 75-85%; the first filler comprises 7-9 parts by weight of silica micropowder with D50 of 10 mu m, 7-9 parts by weight of silica micropowder with D50 of 6 mu m, 33-37 parts by weight of silica micropowder with D50 of 4 mu m, 9-11 parts by weight of silica micropowder with D50 of 2.5 mu m and 4-6 parts by weight of monocrystalline silicon powder with D50 of 1 mu m;
the component B comprises polythiol and a second filler, and the mass fraction of the second filler in the component B is 55-70%; the second filler comprises, by weight, 14-16 parts of monocrystalline silicon powder with a D50 of 4 mu m, 18-22 parts of monocrystalline silicon powder with a D50 of 2 mu m and 18-22 parts of monocrystalline silicon powder with a D50 of 500 nm.
2. The epoxy glue of claim 1, wherein the first filler further comprises titanium dioxide, and wherein the mass ratio of silica, monocrystalline silicon powder and titanium dioxide in the first filler is 61:5:15.
3. The epoxy resin adhesive according to claim 2, wherein the a component further comprises a reactive diluent and fumed silica, and the a component comprises the following components in mass percent: 11-20% of epoxy resin, 75-85% of first filler, 3.5-5% of reactive diluent and 0.1-0.3% of fumed silica.
4. The epoxy resin adhesive of claim 1, wherein the second filler further comprises titanium white, and the mass ratio of the monocrystalline silicon powder to the titanium white in the second filler is 50-60:10-20.
5. The epoxy resin adhesive according to claim 4, wherein the B component further comprises an accelerator and fumed silica, and the B component comprises the following components in mass percent: 20-35% of polythiol, 55-70% of second filler, 7-10% of accelerator and 0.1-0.3% of aerosil.
6. The epoxy resin glue of any one of claims 1 to 5, wherein the first filler and the second filler are both surface modified with a coupling agent selected from titanate coupling agents in an amount of 0.5 to 1% of the filler and silane coupling agents in an amount of 2 to 5% of the filler.
7. The method for preparing the epoxy resin adhesive according to any one of claims 1 to 6, comprising: and respectively mixing and dispersing the raw materials of the component A and the component B, and then mixing the component A and the component B.
8. Use of the epoxy glue of any one of claims 1-6 for bonding silicon rods.
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|---|---|---|---|---|
| JP2002069416A (en) * | 2000-08-31 | 2002-03-08 | Matsushita Electric Ind Co Ltd | Adhesive for electronic component |
| JP2015093916A (en) * | 2013-11-12 | 2015-05-18 | 信越化学工業株式会社 | Conductive epoxy resin composition, solar battery cell using the composition and method for producing the solar battery cell |
| CN112625218A (en) * | 2020-12-17 | 2021-04-09 | 成都硅宝科技股份有限公司 | Epoxy resin for cutting water-resistant silicon rod 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 |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002069416A (en) * | 2000-08-31 | 2002-03-08 | Matsushita Electric Ind Co Ltd | Adhesive for electronic component |
| JP2015093916A (en) * | 2013-11-12 | 2015-05-18 | 信越化学工業株式会社 | Conductive epoxy resin composition, solar battery cell using the composition and method for producing the solar battery cell |
| CN112625218A (en) * | 2020-12-17 | 2021-04-09 | 成都硅宝科技股份有限公司 | Epoxy resin for cutting water-resistant silicon rod 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 |
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