Epoxy resin composition for 940 nm chip, preparation method therefor, and use thereof

Abstract

The present invention relates to the technical field of the preparation for electronic elements, in particular to an epoxy resin composition for a 940 nm chip, a preparation method therefor, and a use thereof. The epoxy resin composition comprises the following components in parts by weight: 60-100 parts of an epoxy resin, 30-65 parts of a curing agent, 0.5-2 parts of a catalyst, and 0.1-15 parts of a dye, wherein the weight ratio of the dye to the curing agent is 1:(3-10). The epoxy resin composition has higher reliability and can withstand three instances of reflow soldering at 260°C, 100 to 500 cycles of high- and low-temperature cycling at -40°C (30 minutes) to 100°C (30 minutes), boiling in red ink at 100°C for 1 hour, and exposure to 85°C and 85% humidity for 1000 hours, without the occurrence of adhesive cracking or lamp failure. The dye and the curing agent are uniformly mixed first to obtain a colorant masterbatch, and the colorant masterbatch is then mixed with the epoxy resin. The use of a solvent is avoided, the melting time is shortened, and the problem that a colorant shows color fading under a high-temperature condition for a long time is also solved.

Description

An epoxy resin composition for 940nm chips and its preparation method and application Technical Field

[0001] The present invention relates to the technical field of electronic component preparation, and more specifically, to an epoxy resin composition for a 940nm chip, a preparation method thereof, and an application thereof. Background Art

[0002] With the widespread use of devices such as smartphones, home appliances, and communications equipment, and the increasing number of remote control applications involving infrared remote control receivers, the frequency of trials under various interference conditions is increasing, especially in light interference environments. This has necessitated improvements in the anti-interference performance of infrared receivers. Currently, epoxy resin molding compounds, with their excellent heat resistance, adhesion, and impact resistance, have been widely used. The use of dyes is unavoidable, and commonly used dyes on the market, such as functional dyes, acid dyes, reactive dyes, and vat dyes, have high transmittance at 400-750nm and low transmittance at 920-1000nm. Infrared receivers encapsulated with such materials have poor anti-interference capabilities and low sensitivity. Therefore, finding dyes that can improve the anti-interference capabilities of infrared receivers is a challenge that needs to be addressed in this field. CN 110951213 A discloses a sunlight-resistant infrared receiver packaging material and its preparation method. The material comprises a first packaging material and a second packaging material. The weight ratio of the first packaging material is: epoxy resin A: epoxy resin B: colorant = 100:100:27-33; the weight ratio of the second packaging material is: epoxy resin A: epoxy resin B: colorant = 100:100:45-55. The infrared receiver packaging material, prepared using epoxy resin as the primary raw material, utilizes the excellent heat and cold resistance inherent in epoxy resin. The colorant is black, and the transmittance of light of different wavelengths has not been studied, resulting in poor anti-interference and sensitivity. Summary of the Invention

[0003] The first aspect of the present invention provides an epoxy resin composition for a 940nm chip, which comprises, 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).

[0004] Direct dyes have poor solubility in epoxy resins. Even after melting at 150-180°C for 2 hours, some dye particles remain undissolved. The applicant has discovered that dissolving direct dyes in a curing agent, particularly tetrahydrophthalic anhydride, not only improves the dispersibility of the dyes but also avoids the use of acetone, dichloromethane, ethanol, or other organic solvents to dissolve the dyes, thereby reducing their toxic effects on the human body.

[0005] Further research found that the weight ratio of dye to curing agent is 1: (3-10), which can be used in the packaging material of infrared receiving elements to effectively improve the anti-interference performance, so that the transmittance at a wavelength of 400-750nm is less than 1%, and the transmittance at a wavelength of 920-1000nm is not less than 80%.

[0006] The curing agent includes at least one of tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, methyl dinac anhydride, methyltetrahydrophthalic anhydride, and hexahydrophthalic anhydride.

[0007] Preferably, the curing agent includes at least one of tetrahydrophthalic anhydride and methylhexahydrophthalic anhydride.

[0008] More preferably, the curing agent includes tetrahydrophthalic anhydride.

[0009] The applicant has discovered that the epoxy resin comprises epoxy resin 1 and epoxy resin 2, wherein epoxy resin 1 comprises a bisphenol A epoxy resin and epoxy resin 2 comprises a glycidyl ester epoxy resin. This can effectively improve the high and low temperature stability and reliability of the material, possibly due to the formation of a specific cross-linked network between the benzene ring structure and the fatty chain. This increases the cross-linking density of the system while maintaining a certain toughness between the molecular chains, thus avoiding volume shrinkage caused by temperature changes. Further research has found that the weight ratio of epoxy resin 1 to epoxy resin 2 is (2-9):1, which can further promote the dispersion of dyes. This is likely due to the formation of hydrogen bonds between the various epoxy resins and dyes having groups such as -SO3Na and -COONa.

[0010] The epoxy resin includes epoxy resin 1 and epoxy resin 2. The epoxy resin 1 includes bisphenol A epoxy resin, and the epoxy resin 2 includes glycidyl ester epoxy resin.

[0011] The epoxy equivalent of the epoxy resin 2 is 50-200 g / eq.

[0012] Preferably, the epoxy resin 2 is purchased from Nissan Chemical, model: Tepic-s.

[0013] The epoxy equivalent of the epoxy resin 1 is 500-100 g / eq and the softening point is 60-100°C.

[0014] Preferably, the epoxy resin 1 is purchased from Sinopec, model: CYD-012.

[0015] The weight ratio of the epoxy resin 1 to the epoxy resin 2 is (2-9):1.

[0016] The catalyst includes at least one of PN-40, 2E4MZ (2-ethyl-4-methylimidazole), MY-25, BDMA (N,N-dimethylbenzylamine), and DMP-30.

[0017] Preferably, the catalyst includes 2E4MZ (2-ethyl-4-methylimidazole) from Shikoku Chemical and BDMA (N,N-dimethylbenzylamine) from Qihe Chemical.

[0018] The epoxy resin composition further comprises an antioxidant and a coupling agent.

[0019] Preferably, the coupling agent is γ-aminopropyltriethoxysilane; and the antioxidant is pentaerythritol tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate.

[0020] The dye comprises a direct dye, and the dye comprises at least one of -SO3Na and -COONa groups.

[0021] Preferably, the dye comprises at least one of the following structures.

[0022] Further preferably, the dye includes direct dye 1, direct dye 2, direct dye 3, and direct dye 4, and the weight ratio of direct dye 1, direct dye 2, direct dye 3, and direct dye 4 is 1:(0.8-1.2):(0.8-1.2):(0.8-1.2).

[0023] Preferably, the weight ratio of direct dye 1, direct dye 2, direct dye 3, and direct dye 4 is 1:1:1:1.

[0024] Further preferably, the direct dye 1 model is direct blue 2B, with an intensity of 100%; the direct dye 2 model is direct green BE, with an intensity of 100%; the direct dye 3 model is direct fast blue B2RL, with an intensity of 100%; the direct dye 4 model is direct fast black G, with an intensity of 100%, and the direct dyes are purchased from Wenzhou Meirenuo Chemical Co., Ltd.

[0025] A second aspect of the present invention provides a method for preparing an epoxy resin composition for a 940nm chip, comprising the following steps:

[0026] Step 1: Melting the epoxy resin and mixing it with an antioxidant to obtain a mixture 1;

[0027] Step 2: Evenly mix the dye and curing agent to obtain a colorant masterbatch;

[0028] Step 3: The colorant masterbatch is mixed with mixture 1 and heated. After the colorant masterbatch is completely melted under a microscope, mixture 3 is obtained;

[0029] Step 4: Add coupling agent and catalyst to mixture 3 and react to obtain the product.

[0030] A third aspect of the present invention provides an application of an epoxy resin composition for a 940nm chip, which is applied to the packaging of an infrared receiver, comprising the following steps:

[0031] S1, crushing the epoxy resin composition into a cake;

[0032] S2, placing the prepared rubber cake into a molding machine to encapsulate the infrared receiver;

[0033] S3, solidify again after packaging. Beneficial effects:

[0034] 1. The epoxy resin includes epoxy resin 1 and epoxy resin 2, wherein epoxy resin 1 includes bisphenol A epoxy resin and epoxy resin 2 includes glycidyl ester epoxy resin, which can effectively improve the high and low temperature stability and reliability of the material.

[0035] 2. The weight ratio of the epoxy resin 1 to the epoxy resin 2 is (2-9):1, which can further promote the dispersion of the dyes and effectively reduce the transmittance of the material in the visible light band.

[0036] 3. During the preparation process, the dye and curing agent are first mixed evenly to obtain a colorant masterbatch, which is then mixed with the epoxy resin. This can effectively solve the problem of poor dye solubility, while avoiding the use of solvents, shortening the melting time, and preventing the colorant from fading due to long-term exposure to high temperature conditions.

[0037] 4. The weight ratio of the dye to the curing agent is 1:(3-10). When used in the packaging material of the infrared receiving element, it can effectively improve the anti-interference performance, so that the transmittance at a wavelength of 400-750nm is less than 1%, and the transmittance at a wavelength of 920-1000nm is not less than 80%; excessive addition of dye will lead to a decrease in the transmittance at 920-1000nm, and it is difficult to completely melt in tetrahydrophthalic anhydride.

[0038] 5. The epoxy composition prepared in this application has higher reliability than other infrared product plastic packaging materials. It can pass 260°C reflow soldering three times, high and low temperature cycle -40 (30min) ~ 100°C (30min) 100-500 times, boiled in 100°C red ink for 1h, and placed at 85°C and 85% humidity for 1000h without glue cracking or dead light. BRIEF DESCRIPTION OF THE DRAWINGS

[0039] FIG1 is a transmittance curve of the resin sample prepared in Example 1.

[0040] FIG2 is a transmittance curve of the resin sample prepared in Example 2.

[0041] FIG3 is a transmittance curve of the resin sample prepared in Example 3.

[0042] FIG4 is a transmittance curve of the resin sample prepared in Example 4.

[0043] FIG5 is a transmittance curve of the resin sample prepared in Example 5.

[0044] FIG6 is a transmittance curve of the resin sample prepared in Example 6.

[0045] FIG7 is a transmittance curve of the resin sample prepared in Example 7.

[0046] FIG8 is a transmittance curve of the resin sample prepared in Comparative Example 1.

[0047] FIG9 is a transmittance curve of the resin sample prepared in Comparative Example 2.

[0048] FIG10 is a transmittance curve of the resin sample prepared in Comparative Example 3.

[0049] FIG11 is a microscope view of the incomplete melting of the dye in Example 1.

[0050] FIG12 is a microscope view of the complete melting of the dye in Example 1.

[0051] FIG13 is a sample prepared in Example 1.

[0052] FIG14 is a bracket molded using the sample prepared in Example 1. DETAILED DESCRIPTION

[0053] Examples and Comparative Examples

[0054] An epoxy resin composition for a 940nm chip, with specific components and amounts in parts by weight as shown in Table 1.

[0055] Table 1 Note: In Table 1, \ indicates that the content of this substance is 0.

[0056] The components are further added with a coupling agent and an antioxidant; the coupling agent is gamma-aminopropyltriethoxysilane; and the antioxidant is pentaerythritol tetrakis[beta-(3,5-di-tert-butyl-4-hydroxyphenyl)propionate].

[0057] The epoxy resin 2 was purchased from Nissan Chemical, model: Tepic-s.

[0058] The epoxy resin 1 was purchased from Sinopec, model: CYD-012.

[0059] The catalyst 1 is 2E4MZ (2-ethyl-4-methylimidazole) from Shikoku Chemical, and the catalyst 2 is BDMA (N,N-dimethylbenzylamine) from Qihe Chemical.

[0060] The dye manufacturers mentioned are all Wenzhou Meirenuo Chemical Co., Ltd.

[0061] The direct dye 1 is direct blue 2B with an intensity of 100%; the direct dye 2 is direct green BE with an intensity of 100%; the direct dye 3 is direct fast blue B2RL with an intensity of 100%; and the direct dye 4 is direct fast black G with an intensity of 100%.

[0062] The model of the reactive dye 1 is Reactive Blue ER 100%; the model of the reactive dye 2 is Reactive Blue EG 100%; the model of the reactive dye 3 is Reactive Blue CE 100%; and the model of the reactive dye 4 is Reactive Black CE 100%.

[0063] The model of acid dye 1 is Acid Blue A-2G Acid Blue 40; the model of acid dye 2 is Weak Acid (Chailin) ​​Brilliant Blue 6B Acid Blue 83; the model of acid dye 3 is Acid Blue SRL Acid Blue 335; and the model of acid dye 4 is Acid Black NT Acid Black 210.

[0064] A method for preparing an epoxy resin composition for a 940nm chip comprises the following steps:

[0065] Step 1: Melt the epoxy resin. Weigh epoxy resin 1, epoxy resin 2, and antioxidant in a beaker and heat at 180°C for 50 minutes. After the epoxy resin and antioxidant are completely melted, proceed to the next step.

[0066] Step 2: After the curing agent is melted under reduced pressure in a flask, the dye is added and stirred using a dispersion plate at a speed of 500 rpm for 4 minutes to uniformly disperse the dye in the tetrahydrophthalic anhydride to prepare a colorant masterbatch;

[0067] Step 3: Take out the colorant masterbatch prepared in step 2 and place it in the mixture of step 1. Heat it at 90°C for 20 minutes and observe the melting process. The part that is not completely melted is shown in Figure 11. The colorant masterbatch is completely melted under a microscope, as shown in Figure 12. Then proceed to the next step.

[0068] Step 4: Add coupling agent and catalyst to the mixture of step 3 and react to obtain the product.

[0069] An application of an epoxy resin composition for a 940nm chip, which is applied to the packaging of an infrared receiver, comprises the following steps:

[0070] S1, crushing the epoxy resin composition into a cake;

[0071] S2, the prepared rubber cake is placed in a molding machine to encapsulate the infrared receiver (the encapsulated sample is shown in Figure 14, corresponding to the application of the composition obtained in Example 1);

[0072] S3, after packaging, cure again at 150°C for 4h.

[0073] Performance testing methods

[0074] The samples prepared in the examples and comparative examples were subjected to performance tests. The test data of the examples are listed in Table 2, and the test data of the comparative examples are listed in Table 3.

[0075] Light transmittance: The epoxy resin compositions prepared in Examples 1 to 7 and Comparative Examples 1 to 3 were crushed and beaten into cakes. The cakes were pressed at 150° C. for 5 min to obtain 0.3 mm thick samples (see FIG13 for examples of the samples). The light transmittance of the samples was tested over the entire wavelength range of 400-1000 nm, as shown in FIG1 to FIG10 .

[0076] Reliability test: reflow soldering at 260℃ for three times. If there is no glue cracking or dead light, it is qualified and recorded as OK. Otherwise, it fails and is recorded as NO.

[0077] High and low temperature cycle times: first -40℃ (30min), then 100℃ (30min), cycle 100-500 times. If there is no glue cracking or dead light, it is qualified and recorded as OK. Otherwise, it is unqualified and recorded as NO.

[0078] Boiling resistance: Boil in red ink at 100℃ for 1 hour. If there is no glue cracking or dead light, it is qualified and recorded as OK. Otherwise, it is unqualified and recorded as NO.

[0079] [Corrected 10.12.2024 according to Rule 26] High temperature and high humidity performance: After being placed at 85℃ and 85% humidity for 1000h, if there is no glue cracking or dead light, it is qualified and recorded as OK; otherwise it is unqualified and recorded as NO.

[0080] Performance test data

[0081] Table 2

[0082] Table 3

Claims

1. An epoxy resin composition for 940nm chip, characterized in that, Calculated by weight, the components include: 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).

2. An epoxy resin composition for 940nm chip according to claim 1, characterized in that: The curing agent includes at least one of tetrahydrophthalic anhydride, methylhexahydrophthalic anhydride, methyl dinac anhydride, methyltetrahydrophthalic anhydride and hexahydrophthalic anhydride.

3. An epoxy resin composition for 940nm chip according to claim 2, characterized in that: The epoxy resin includes epoxy resin 1 and epoxy resin 2. The epoxy resin 1 includes bisphenol A type epoxy resin, and the epoxy resin 2 includes glycidyl ester type epoxy resin.

4. The epoxy resin composition for 940nm chip according to claim 3, characterized in that: The epoxy equivalent of the epoxy resin 2 is 50-200 g / eq.

5. The epoxy resin composition for 940nm chip according to claim 4, characterized in that: The epoxy equivalent of the epoxy resin 1 is 500-100 g / eq and the softening point is 60-100°C.

6. The epoxy resin composition for 940nm chip according to claim 5, characterized in that: The catalyst includes at least one of PN-40, 2E4MZ, MY-25, BDMA, and DMP-30.

7. An epoxy resin composition for 940nm chip according to claim 1 or 6, characterized in that: The epoxy resin composition further comprises an antioxidant and a coupling agent.

8. The epoxy resin composition for 940nm chip according to claim 7, characterized in that: The dye comprises a direct dye, and the dye comprises at least one of -SO3Na and -COONa groups.

9. A method for preparing the epoxy resin composition for 940nm chip according to claim 7 or 8, comprising the following steps: Step 1: Melting the epoxy resin and mixing it with an antioxidant to obtain a mixture 1; Step 2: Evenly mix the dye and the curing agent to obtain a colorant masterbatch; Step 3: The colorant masterbatch is mixed with the mixture 1 and heated, and after the colorant masterbatch is observed to be completely melted under a microscope, a mixture 3 is obtained; Step 4: Add coupling agent and catalyst to mixture 3 and obtain the product after reaction.

10. An application of the epoxy resin composition for 940nm chips according to any one of claims 1 to 8, characterized in that: The packaging for the infrared receiver includes the following steps: S1, crushing the epoxy resin composition into a rubber cake; S2, putting the prepared rubber cake into a molding machine to encapsulate the infrared receiver; S3, solidify again after packaging.

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