CN117264378B - Epoxy resin composition for 940nm chip and preparation method and application thereof - Google Patents

Epoxy resin composition for 940nm chip and preparation method and application thereof Download PDF

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Publication number
CN117264378B
CN117264378B CN202311573306.1A CN202311573306A CN117264378B CN 117264378 B CN117264378 B CN 117264378B CN 202311573306 A CN202311573306 A CN 202311573306A CN 117264378 B CN117264378 B CN 117264378B
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epoxy resin
dye
resin composition
direct
direct dye
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CN117264378A (en
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杨岚
单秋菊
孙绪筠
谭晓华
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Tianjin Degao Huacheng Optoelectronics Technology Co ltd
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Tianjin Degao Huacheng Optoelectronics Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/20Compounding polymers with additives, e.g. colouring
    • C08J3/22Compounding polymers with additives, e.g. colouring using masterbatch techniques
    • C08J3/223Packed additives
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K5/00Casings, cabinets or drawers for electric apparatus
    • H05K5/06Hermetically-sealed casings
    • H05K5/065Hermetically-sealed casings sealed by encapsulation, e.g. waterproof resin forming an integral casing, injection moulding
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • C08L2203/206Applications use in electrical or conductive gadgets use in coating or encapsulating of electronic parts

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Epoxy Resins (AREA)

Abstract

The invention relates to the technical field of electronic element preparation, in particular to an epoxy resin composition for a 940nm chip, and a preparation method and application thereof. The components in parts by weight are as follows: 60-100 parts of epoxy resin, 30-65 parts of curing agent, 0.5-2 parts of catalyst and 0.1-15 parts of dye; the weight ratio of the dye to the curing agent is 1: (3-10). The high reliability can be achieved by three times of reflow soldering at 260 ℃, high and low temperature circulation is carried out for-40 (30 min) to 100 ℃ (30 min) for 100-500 times, the high and low temperature circulation is carried out for 1h in red ink at 100 ℃, the high and low temperature circulation is carried out for 1000h at 85 ℃ under 85% humidity, and no glue crack and lamp death occur. The dye and the curing agent are uniformly mixed to obtain the color master batch, and then the color master batch is mixed with the epoxy resin, so that the use of a solvent is avoided, the melting time is shortened, and the problem of fading of the color is avoided when the color is in a high temperature condition for a long time.

Description

Epoxy resin composition for 940nm chip and preparation method and application thereof
Technical Field
The invention relates to the technical field of electronic element preparation, in particular to an epoxy resin composition for a 940nm chip, and a preparation method and application thereof.
Background
With the wide application of smart phones, home appliances, communication equipment and other devices, and the increasing number of remote control fields related to infrared remote control receivers, the trial frequency under different interference conditions is increased, and particularly, the working condition under the interference environment of light is increased, so that the anti-interference performance of the infrared remote control receivers needs to be improved. At present, the epoxy resin plastic package material has been widely used in terms of excellent heat resistance, adhesion and impact resistance. The dyes can not be avoided, but the dyes commonly used in the market at present, such as functional dyes, acid dyes, reactive dyes and vat dyes, have higher transmittance at 400-750nm and lower transmittance at 920-1000nm, and the infrared receiver packaged by the material has poorer anti-interference capability and lower sensitivity, so that the finding of the dyes capable of improving the anti-interference capability of the infrared receiver is a problem to be solved in the field.
CN 110951213A discloses a solar-resistant infrared receiver packaging material and a preparation method thereof, the packaging material comprises a packaging material I and a packaging material II, wherein the weight ratio of the packaging material I is as follows: epoxy resin A material: epoxy resin B material: pigment=100:100:27-33, and the weight ratio of the second packaging material is as follows: epoxy resin A material: epoxy resin B material: colorant=100:100:45-55. The infrared receiver packaging material prepared by using the epoxy resin as a main raw material has good heat resistance and cold resistance of the epoxy resin. The coloring material is black, has not been studied on transmittance of light with different wavelengths, and has not excellent anti-interference and sensitivity.
Disclosure of Invention
The first aspect of the invention provides an epoxy resin composition for 940nm chips, which comprises the following components in parts by weight: 60-100 parts of epoxy resin, 30-65 parts of curing agent, 0.5-2 parts of catalyst and 0.1-15 parts of dye; the weight ratio of the dye to the curing agent is 1: (3-10).
The present inventors have found that the dissolution of the direct dye in a curing agent, particularly tetrahydrophthalic anhydride, not only improves the dispersion properties of the dye, but also avoids the use of acetone, methylene dichloride, ethanol or other organic solvents as solvents to dissolve the dye, thereby reducing the toxic effects on human bodies.
Further studies have found that the weight ratio of dye to curing agent is 1: (3-10) is applied to the packaging material of the infrared receiving element, and can effectively improve the anti-interference performance, so that the infrared receiving element has the transmittance of less than 1% at the wavelength of 400-750nm, and has the transmittance of not less than 80% at the wavelength of 920-1000 nm.
The curing agent comprises at least one of tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride, methyl diAN_SNhan, methyl tetrahydrophthalic anhydride and hexahydrophthalic anhydride.
Preferably, the curing agent comprises at least one of tetrahydrophthalic anhydride and methyl hexahydrophthalic anhydride.
Further preferably, the curing agent comprises tetrahydrophthalic anhydride.
The present inventors have found that the epoxy resin includes an epoxy resin 1 and an epoxy resin 2, the epoxy resin 1 includes a bisphenol a type epoxy resin, and the epoxy resin 2 includes a glycidyl ester type epoxy resin. The high-low temperature stability and the reliability of the material can be effectively improved, a specific cross-linking network is possibly formed between a benzene ring structure and a fatty chain, certain toughness exists between molecular chains while the cross-linking density of the system is improved, and the volume shrinkage caused by temperature change is avoided, and further research shows that the weight ratio of the epoxy resin 1 to the epoxy resin 2 is (2-9): 1, further promoting the dispersion of the dyes, possibly hydrogen bonds between various epoxy resins and dyes having groups such as-SO 3 Na and-COONa, etc.
The epoxy resin includes an epoxy resin 1 and an epoxy resin 2, the epoxy resin 1 includes a bisphenol a type epoxy resin, and the epoxy resin 2 includes a glycidyl ester type epoxy resin.
The epoxy equivalent of the epoxy resin 2 is 50-200g/eq.
Preferably, the epoxy resin 2 is available from Nissan Chemie, model: tepic-s.
The epoxy equivalent of the epoxy resin 1 is 500-100g/eq, and the softening point is 60-100 ℃.
Preferably, the epoxy resin 1 is purchased from medium petrochemical, model: CYD-012.
The weight ratio of the epoxy resin 1 to the epoxy resin 2 is (2-9): 1.
The catalyst comprises at least one of PN-40, 2E4MZ (2-ethyl-4-methylimidazole), MY-25, BDMA (N, N-dimethylbenzylamine) and DMP-30.
Preferably, the catalyst comprises tetradentate 2E4MZ (2-ethyl-4-methylimidazole) and haloxyfop chemical BDMA (N, N-dimethylbenzylamine).
The epoxy resin composition further includes an antioxidant and a coupling agent.
Preferably, the coupling agent is gamma-aminopropyl triethoxysilane; the antioxidant is pentaerythritol tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
The dye includes a direct type dye including at least one of-SO 3 Na and-COONa groups.
Preferably, the dye comprises at least one of the following structures.
Further preferably, the dye comprises a direct dye 1, a direct dye 2, a direct dye 3 and a direct dye 4, wherein the weight ratio of the direct dye 1, the direct dye 2, the direct dye 3 and the direct dye 4 is 1: (0.8-1.2): (0.8-1.2): (0.8-1.2).
Preferably, the direct dye 1, the direct dye 2, the direct dye 3 and the direct dye 4 have the weight ratio of 1:1: 1:1.
Further preferably, the direct dye 1 is direct blue 2B with 100% strength; the direct dye 2 is direct green BE with 100% strength; the direct dye 3 is direct fast blue B2RL with the intensity of 100 percent; the direct dye type 4 is direct suntan G, 100% strength, and is purchased from melno chemical company, wenzhou.
The second aspect of the present invention provides a method for preparing an epoxy resin composition for 940nm chips, comprising the steps of:
Step 1: melting epoxy resin, and mixing with an antioxidant to obtain a mixture 1;
step 2: uniformly mixing the dye and the curing agent to obtain a toner mother adhesive;
step 3: mixing and heating the color master batch and the mixture 1, and observing that the color master batch is completely melted under a microscope to obtain a mixture 3;
Step 4: adding a coupling agent and a catalyst into the mixture 3, and reacting to obtain the catalyst.
In a third aspect, the present invention provides an application of an epoxy resin composition for 940nm chips, applied to packaging of an infrared receiver, comprising the steps of:
s1, crushing the epoxy resin composition and then beating into a rubber cake;
s2, placing the prepared rubber cake into a molding press, and packaging an infrared receiver;
S3, packaging and then curing again.
The beneficial effects are that:
1. the epoxy resin comprises epoxy resin 1 and epoxy resin 2, wherein the epoxy resin 1 comprises bisphenol A epoxy resin, and the epoxy resin 2 comprises glycidyl ester epoxy resin, so that the high-low temperature stability and the reliability of the material can be effectively improved.
2. The weight ratio of the epoxy resin 1 to the epoxy resin 2 is (2-9): 1, the dispersion among the dyes can be further promoted, and the light transmittance of the material in the visible light wave band range is effectively reduced.
3. In the preparation process, the dye and the curing agent are uniformly mixed to obtain the color agent masterbatch, and then the color agent masterbatch is mixed with the epoxy resin, so that the problem of poor solubility of the dye can be effectively solved, the use of a solvent is avoided, the melting time is shortened, and the problem of fading of the color agent under the condition of high temperature for a long time is also avoided.
4. The weight ratio of the dye to the curing agent is 1: (3-10) the anti-interference performance can be effectively improved by being applied to the packaging material of the infrared receiving element, so that the infrared receiving element has the transmittance of less than 1% at the wavelength of 400-750nm and the transmittance of not less than 80% at the wavelength of 920-1000 nm; too much dye addition results in a decrease in light transmittance at 920-1000nm and difficulty in complete melting in tetrahydrophthalic anhydride.
5. Compared with other infrared product plastic packaging materials, the epoxy composition prepared by the application has higher reliability, can be subjected to reflow soldering for three times at 260 ℃, has high and low temperature circulation of-40 (30 min) to 100 ℃ (30 min) for 100-500 times, is boiled in red ink at 100 ℃ for 1h, is placed at 85 ℃ under the humidity of 85% for 1000h, and has no glue crack and lamp death.
Drawings
FIG. 1 is a graph showing the transmittance of the resin sample prepared in example 1.
FIG. 2 is a graph showing the transmittance of the resin sample prepared in example 2.
FIG. 3 is a graph showing the transmittance of the resin sample prepared in example 3.
FIG. 4 is a graph showing the transmittance of the resin sample prepared in example 4.
FIG. 5 is a graph showing the transmittance of the resin sample prepared in example 5.
FIG. 6 is a graph showing the transmittance of the resin sample prepared in example 6.
FIG. 7 is a graph showing the transmittance of the resin sample prepared in example 7.
FIG. 8 is a graph showing the transmittance of the resin sample prepared in comparative example 1.
FIG. 9 is a graph showing the transmittance of the resin sample prepared in comparative example 2.
FIG. 10 is a graph showing the transmittance of the resin sample prepared in comparative example 3.
FIG. 11 is a view of a microscope with dye not fully melted in example 1.
FIG. 12 is a view of a full melt microscope of the dye of example 1.
FIG. 13 is a sample wafer prepared in example 1.
FIG. 14 is a molded stent using the coupon prepared in example 1.
Detailed Description
Examples and comparative examples
The epoxy resin composition for 940nm chip has the specific components and amounts shown in Table 1 in parts by weight.
TABLE 1
Note that: table 1 shows that the content of this substance is 0.
The components are also added with a coupling agent and an antioxidant; the coupling agent is gamma-aminopropyl triethoxysilane; the antioxidant is pentaerythritol tetra [ beta- (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate ].
The epoxy resin 2 was purchased from daily chemical, model: tepic-s.
The epoxy resin 1 is purchased from medium petrochemical industry, model: CYD-012.
The catalyst 1 is formed by four countries, namely 2E4MZ (2-ethyl-4-methylimidazole), and the catalyst 2 is formed by BDMA (N, N-dimethylbenzylamine) in the chemical industry of Qihe grass.
The dye manufacturers are all Winnuo chemical industry Co., ltd.
The direct dye 1 is direct blue 2B, and the strength is 100%; the direct dye 2 is direct green BE with 100% strength; the direct dye 3 is direct fast blue B2RL with the intensity of 100 percent; the direct dye type 4 was direct suntan G, 100% strength.
The type 1 Reactive dye is Reactive Blue E-R100%; reactive dye 2 is the Reactive Blue E-G100%; reactive dye 3 is 100% of Reactive Blue CE; the type number of the reactive dye 4 is Reactive Black CE percent.
The model 1 of the Acid dye is Acid Blue A-2G Acid Blue 40; the model 2 of the acid dye is weak acid (Chailin) brilliant Blue 6BAcid Blue 83; acid dye 3 is Acid Blue SRL Acid Blue 335; acid dye 4 is Acid Black NT Acid Black 210.
A preparation method of an epoxy resin composition for 940nm chips comprises the following steps:
Step 1: melting epoxy resin, weighing epoxy resin 1, epoxy resin 2 and antioxidant in a beaker, heating at 180 ℃ for 50min, and carrying out the next step after the epoxy resin and the antioxidant are completely melted;
Step 2: after the curing agent is decompressed and melted in a flask, adding the dye, stirring by using a dispersing disc at the rotating speed of 500rpm for 4min to ensure that the dye is uniformly dispersed in tetrahydrophthalic anhydride, and preparing the color former masterbatch;
Step 3: taking out the color master batch prepared in the step 2, placing the color master batch in the mixture in the step 1, heating the mixture at 90 ℃ for 20min, observing a melting process, wherein the color master batch is not completely melted as shown in fig. 11, observing that the color master batch is completely melted under a microscope as shown in fig. 12, and performing the next operation;
Step 4: and (3) adding a coupling agent and a catalyst into the mixture obtained in the step (3), and reacting to obtain the catalyst.
An application of an epoxy resin composition for 940nm chips, which is applied to packaging of an infrared receiver, comprises the following steps:
s1, crushing the epoxy resin composition and then beating into a rubber cake;
S2, placing the prepared rubber cake into a molding press, and packaging an infrared receiver (a packaged sample is shown in FIG. 14 and corresponds to the application of the composition obtained in the example 1);
S3, after packaging, curing for 4 hours at 150 ℃.
Performance test method
The samples prepared in examples and comparative examples were subjected to performance testing, the example test data are listed in table 2, and the comparative example test data are listed in table 3.
Transmittance: taking the epoxy resin compositions prepared in examples 1-7 and comparative examples 1-3, crushing, and then beating into a rubber cake, and performing film pressing at 150 ℃ for 5min to obtain a sample sheet with the thickness of 0.3mm (sample sheet example is shown in figure 13), wherein the light transmittance of the test sample sheet in the whole wave band of 400-1000nm is shown in figures 1-10.
Reliability test: reflow soldering is carried out for three times at 260 ℃, the situation that NO glue cracks and lamp death occur is qualified, the condition is marked as OK, otherwise, the condition is unqualified, and the condition is marked as NO;
High and low temperature cycle times: firstly, performing-40 ℃ (30 min), then performing 100 ℃ (30 min), and circulating for 100-500 times, wherein the condition of NO glue crack and lamp death appears as qualified, and is marked as OK, otherwise, the condition of NO glue crack and lamp death does not appear as unqualified, and is marked as NO;
Boiling resistance: boiling in 100 ℃ red ink for 1h, wherein NO glue crack and lamp death appear as qualified, and marking as OK, otherwise, unqualified, and marking as NO;
High temperature and high humidity performance: placing at 85deg.C and humidity of 85% for 1000 hr, and marking as OK if NO glue crack or lamp death occurs, or else, marking as NO if NO glue crack or lamp death occurs;
Performance test data
TABLE 2
TABLE 3 Table 3

Claims (9)

1. An epoxy resin composition for 940nm chips is characterized by comprising the following components in parts by weight: 60-100 parts of epoxy resin, 30-65 parts of curing agent, 0.5-2 parts of catalyst and 0.1-15 parts of dye; the weight ratio of the dye to the curing agent is 1: (3-10);
The dye comprises a direct dye 1, a direct dye 2, a direct dye 3 and a direct dye 4;
The direct dye 1, the direct dye 2, the direct dye 3 and the direct dye 4 are in a weight ratio of 1: (0.8-1.2): (0.8-1.2): (0.8-1.2);
The direct dye 1 is direct blue 2B, and the strength is 100%; the direct dye 2 is direct green BE with 100% strength; the direct dye 3 is direct fast blue B2RL with the intensity of 100 percent; the direct dye type 4 is direct suntan G, and the strength is 100%;
The direct dye was purchased from melno chemical company, wenzhou.
2. An epoxy resin composition for 940nm chips according to claim 1, wherein the curing agent comprises at least one of tetrahydrophthalic anhydride, methyl hexahydrophthalic anhydride, methyl di-sodium gram anhydride, methyl tetrahydrophthalic anhydride, hexahydrophthalic anhydride.
3. An epoxy resin composition for 940nm chips according to claim 2, wherein the epoxy resin comprises an epoxy resin 1 and an epoxy resin 2, the epoxy resin 1 comprises a bisphenol a type epoxy resin, and the epoxy resin 2 comprises a glycidyl ester type epoxy resin.
4. An epoxy resin composition for 940nm chip according to claim 3, wherein the epoxy equivalent of the epoxy resin 2 is 50-200g/eq.
5. The epoxy resin composition for 940nm chip according to claim 4, wherein the epoxy resin 1 has an epoxy equivalent of 500 to 100g/eq and a softening point of 60 to 100 ℃.
6. The epoxy resin composition for 940nm chips according to claim 5, wherein the catalyst comprises at least one of PN-40, 2E4MZ, MY-25, BDMA, DMP-30.
7. An epoxy resin composition for 940nm chips according to claim 1 or 6, wherein the epoxy resin composition further comprises an antioxidant and a coupling agent.
8. A method for preparing the epoxy resin composition for 940nm chips according to claim 7, comprising the steps of:
Step 1: melting epoxy resin, and mixing with an antioxidant to obtain a mixture 1;
step 2: uniformly mixing the dye and the curing agent to obtain a toner mother adhesive;
step 3: mixing and heating the color master batch and the mixture 1, and observing that the color master batch is completely melted under a microscope to obtain a mixture 3;
Step 4: adding a coupling agent and a catalyst into the mixture 3, and reacting to obtain the catalyst.
9. Use of an epoxy resin composition for 940nm chips according to any of claims 1-6, for packaging of infrared receivers, comprising the steps of:
s1, crushing the epoxy resin composition and then beating into a rubber cake;
s2, placing the prepared rubber cake into a molding press, and packaging an infrared receiver;
S3, packaging and then curing again.
CN202311573306.1A 2023-11-23 2023-11-23 Epoxy resin composition for 940nm chip and preparation method and application thereof Active CN117264378B (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104693689A (en) * 2015-04-08 2015-06-10 天津盛远达科技有限公司 Epoxy molding compound for infrared receiver module and preparing method of epoxy molding compound
CN114806054A (en) * 2021-12-14 2022-07-29 南京聚隆科技股份有限公司 Infrared-transmitting anti-scratch master batch, and preparation method and application thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104693689A (en) * 2015-04-08 2015-06-10 天津盛远达科技有限公司 Epoxy molding compound for infrared receiver module and preparing method of epoxy molding compound
CN114806054A (en) * 2021-12-14 2022-07-29 南京聚隆科技股份有限公司 Infrared-transmitting anti-scratch master batch, and preparation method and application thereof

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