Packaging ink, preparation method and application thereof, device and equipment

By blending silicone epoxy resin and core-shell phenolic epoxy prepolymer, the composition and process of the packaging ink are optimized, the structural density and weather resistance problems of the ink protective coating are solved, higher stability and tolerance are achieved, and the resistance performance of semiconductor packaging is improved.

CN118109075BActive Publication Date: 2025-10-03JIANGSU AISEN SEMICON MATERIAL CO LTD +1
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Patent Information

Application Number
CN202410222597.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-02-28
Publication Date
2025-10-03
Estimated Expiration
2044-02-28

AI Technical Summary

Technical Problem

In existing semiconductor packaging structures, the ink protective coating of chip resistors has problems such as poor structural density and poor weather resistance, which leads to the intrusion of sulfur and sulfides and poor adhesion, affecting the stability and service life of the resistors.

Method used

A silicone epoxy resin and a core-shell phenolic epoxy prepolymer are blended to optimize the composition and process of the encapsulated ink, improve the stability and tolerance of the ink, and prepare the ink through stirring, dispersing, grinding and filtering.

Benefits of technology

It significantly improves the ink's resistance to cold and heat shock, water resistance, and resistance to folding and cracking, enhances the ink's application performance, and ensures the product's service life and stability.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention provides an encapsulation ink, its preparation method, application, device, and equipment. The raw materials for preparing the encapsulation ink include the following components by weight: 20 to 35 parts of a first epoxy resin, 1 to 10 parts of a second epoxy resin, 3 to 7 parts of a curing agent, 0.15 to 7 parts of a curing accelerator, and 10 to 35 parts of a filler; wherein the first epoxy resin includes a silicone-type epoxy resin and a core-shell phenolic epoxy prepolymer; wherein the second epoxy resin includes a phenolic epoxy resin. By optimizing the composition and process of the encapsulation ink, the present invention effectively improves the surface and flexibility of the ink product, thereby meeting the adaptability in the production environment and the application process, and ensuring the performance of the product.
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Description

Technical Field

[0001] The present invention relates to the field of semiconductor packaging technology, and in particular to packaging ink, a preparation method and application thereof, and devices and equipment. Background Art

[0002] To improve the electrical properties of semiconductor packaging structures, passive components such as capacitors, resistors, or inductors are installed in the semiconductor packaging structure. Among them, resistors are generally used for voltage division, current shunting, filtering, and impedance matching. The main type of resistor used is chip resistor (Chip Resistor), also known as chip resistor (SMD Resistor). Chip resistors are a type of metal glass glaze resistor. The resistor is made by printing metal silver paste and glass glaze powder on a substrate using the silk screen printing method, and then a layer of insulating ink protective coating is printed on the outermost layer. Chip resistors can generally be divided into conventional series thick film chip resistors and high-precision and high-stability chip resistors. Among them, conventional series thick film chip resistors are mainly used in general consumer products; high-precision and high-stability chip resistors are mainly used in medical equipment, precision measuring instruments, electronic communications, automotive equipment, etc.

[0003] The rapid development of the integrated circuit industry is driving increasingly higher performance demands on passive components, particularly high structural density and weather resistance requirements for the protective coatings on high-precision and stable chip resistors. Poor structural density can lead to poor sealing during use. Poor weather resistance can lead to sulfur and water molecules penetrating the packaging ink in the presence of sulfur and sulfides, damaging the resistor. Poor water resistance can also lead to poor adhesion to the substrate during use, causing the ink to fall off.

[0004] In view of this, the present invention is proposed. Summary of the Invention

[0005] One of the objectives of the present invention is to provide an encapsulation ink, wherein the raw materials for preparing the encapsulation ink include the following components by weight: 20-35 parts of a first epoxy resin, 1-10 parts of a second epoxy resin, 3-7 parts of a curing agent, 0.15-7 parts of a curing accelerator, and 10-35 parts of a filler; wherein the first epoxy resin comprises an organosilicon epoxy resin and a core-shell phenolic epoxy prepolymer; and wherein the second epoxy resin comprises a phenolic epoxy resin. By optimizing the composition of the encapsulation ink, the present invention effectively improves the stability and tolerance of the ink product, thereby meeting its adaptability in production environments and applications, and ensuring the product's service life.

[0006] A second object of the present invention is to provide a method for preparing the encapsulation ink, comprising the following steps: mixing the raw materials for the encapsulation ink, stirring and dispersing the raw materials, grinding the raw materials, and filtering the raw materials to obtain the encapsulation ink. By optimizing the encapsulation ink process, the present invention effectively improves the stability and durability of the ink product, thereby meeting its adaptability to production environments and applications, and ensuring the product's service life.

[0007] A third object of the present invention is to provide an application of the packaging ink in semiconductor passive component packaging.

[0008] A fourth object of the present invention is to provide a semiconductor device comprising a deposit formed by the above-mentioned packaging ink.

[0009] A fifth object of the present invention is to provide a device comprising a deposit formed by the encapsulation ink, or a semiconductor device as described above.

[0010] In order to achieve the above-mentioned purpose of the present invention, the following technical solutions are adopted:

[0011] In a first aspect, the present invention provides an ink for packaging, wherein the raw materials for preparing the ink for packaging include the following components in parts by weight:

[0012] 20-35 parts of the first epoxy resin, 1-10 parts of the second epoxy resin, 3-7 parts of the curing agent, 0.15-7 parts of the curing accelerator, and 10-35 parts of the filler;

[0013] Wherein, the first epoxy resin comprises an organosilicon epoxy resin and a core-shell structure phenolic epoxy prepolymer;

[0014] Wherein, the second epoxy resin includes novolac epoxy resin.

[0015] It's important to note that the epoxy group functionality of silicone epoxy resins is greater than 2, while that of standard bisphenol A epoxy resins is 2. Therefore, silicone epoxy coatings have higher crosslink density, toughness, water resistance, and thermal shock resistance than standard bisphenol A epoxy coatings. Silicone epoxy resins are generally not used alone, but rather blended with other resins or prepolymers.

[0016] In the present invention, silicone epoxy resin and core-shell structure phenolic epoxy prepolymer are selected for blending and use because the core-shell structure phenolic epoxy prepolymer has extremely strong toughening effect, reduced water absorption and excellent system dispersibility. By blending these two materials, the resin crystallization can be effectively prevented, the resin fluidity can be improved, and the material dispersion during the processing process can be facilitated. The blending of different epoxy resins also gives the ink excellent resistance to cold and hot shock, water barrier properties and film toughness.

[0017] In the raw materials for preparing the packaging ink, the content of the first epoxy resin is 20 to 35 parts, for example, it can be 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, 26 parts, 27 parts, 28 parts, 29 parts, 30 parts, 31 parts, 32 parts, 33 parts, 34 parts, 35 parts, etc.

[0018] In the raw materials for preparing the packaging ink, the content of the second epoxy resin is 1 to 10 parts, for example, 1 part, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, etc.

[0019] In the raw materials for preparing the packaging ink, the content of the curing agent is 3 to 7 parts, for example, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, etc.

[0020] In the raw materials for preparing the packaging ink, the content of the curing accelerator is 0.15 to 7 parts, for example, it can be 0.15 parts, 0.2 parts, 0.4 parts, 0.6 parts, 0.8 parts, 1 part, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, etc.

[0021] In the raw materials for preparing the packaging ink, the total content of fillers is 10 to 35 parts, for example, it can be 10 parts, 12 parts, 14 parts, 16 parts, 18 parts, 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, 26 parts, 27 parts, 28 parts, 29 parts, 30 parts, 31 parts, 32 parts, 33 parts, 34 parts, 35 parts, etc.

[0022] Preferably, the mass ratio of the silicone epoxy resin to the core-shell novolac epoxy prepolymer is (1-2.5):(1-2.5), for example, it can be 1:1, 1:2.5, 2:1.5, 2:1, 1.5:2, 1:2, 2.5:1, etc.

[0023] Furthermore, in the first epoxy resin, the content of the silicone-based epoxy resin is 10 to 25 parts, for example, 10 parts, 12 parts, 14 parts, 16 parts, 18 parts, 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, etc.

[0024] Furthermore, in the first epoxy resin, the content of the core-shell phenolic epoxy prepolymer is 10 to 25 parts, for example, it can be 10 parts, 12 parts, 14 parts, 16 parts, 18 parts, 20 parts, 21 parts, 22 parts, 23 parts, 24 parts, 25 parts, etc.

[0025] Preferably, the epoxy equivalent of the silicone-based epoxy resin is 230 to 250 g / eq, for example, it can be 230 g / eq, 232 g / eq, 234 g / eq, 236 g / eq, 238 g / eq, 240 g / eq, 242 g / eq, 246 g / eq, 248 g / eq, 250 g / eq, etc.

[0026] Preferably, the rubber content in the core-shell phenolic epoxy prepolymer is 30-45wt%, for example, it can be 30wt%, 32wt%, 34wt%, 36wt%, 38wt%, 40wt%, 42wt%, 45wt%, etc.

[0027] It should be noted that the rubber here refers to the rubber that plays a toughening role in the prepolymer (for example, it can be polybutadiene rubber, nitrile rubber, etc.), and 30-45wt% refers to the mass proportion of the toughening rubber in the core-shell structure phenolic epoxy prepolymer.

[0028] Preferably, the epoxy equivalent of the core-shell structure phenolic epoxy prepolymer is 260-280 g / eq, for example, it can be 260 g / eq, 262 g / eq, 264 g / eq, 266 g / eq, 268 g / eq, 270 g / eq, 272 g / eq, 276 g / eq, 278 g / eq, 280 g / eq, etc.

[0029] Preferably, the epoxy equivalent of the novolac epoxy resin is 185 to 195 g / eq, for example, it can be 185 g / eq, 186 g / eq, 187 g / eq, 188 g / eq, 189 g / eq, 190 g / eq, 191 g / eq, 192 g / eq, 193 g / eq, 194 g / eq, 195 g / eq, etc.

[0030] Preferably, the molecular weight of the novolac epoxy resin is 500-700 g / mol, for example, 500 g / mol, 520 g / mol, 540 g / mol, 560 g / mol, 580 g / mol, 600 g / mol, 620 g / mol, 640 g / mol, 680 g / mol, 700 g / mol, etc.

[0031] Preferably, the total chlorine content of the novolac epoxy resin is ≤1200 ppm, for example, it may be 1200 ppm, 1100 ppm, 1000 ppm, 900 ppm, 800 ppm, 600 ppm, 500 ppm, 400 ppm, 200 ppm, 100 ppm, etc.

[0032] Preferably, the melting temperature of the novolac epoxy resin is less than 90°C, for example, it may be 89°C, 88°C, 87°C, 86°C, 85°C, 84°C, 82°C, 80°C, 75°C, 70°C, etc.

[0033] Preferably, the curing agent is a latent amine curing agent containing active hydrogen.

[0034] Preferably, the amine value of the curing agent is ≥50, for example, it can be 50, 52, 54, 56, 58, 60, etc.

[0035] Preferably, the active hydrogen equivalent of the curing agent is 140-145, for example, 140, 140.5, 141, 141.5, 142, 142.5, 143, 143.5, 144, 144.5, 145, etc.

[0036] Preferably, the latent amine curing agent is selected from any one of dicyandiamide, diaminodiphenyl sulfone or adipic acid dihydrazide, or a combination of at least two thereof.

[0037] Preferably, the curing accelerator is selected from any one of urea accelerators, phenol accelerators, imidazole accelerators or hydrazide accelerators, or a combination of at least two thereof.

[0038] Furthermore, the urea accelerator includes but is not limited to any one or a combination of at least two of N-(2-hydroxyphenyl)-N',N'-dimethylurea, N-(2-hydroxy-4-nitrobenzene)-N',N'-dimethylurea, N-(5-chloro-2-hydroxybenzene)-N',N'-dimethylurea, N-(4-chlorophenyl)-N',N'-dimethylurea or N-(4-chloro-2-hydroxybenzene)-N',N'-dimethylurea.

[0039] Furthermore, the phenolic accelerator includes but is not limited to 2,4,6-tris(dimethylaminomethyl)phenol.

[0040] Furthermore, the imidazole accelerator includes but is not limited to any one or a combination of at least two of 1-benzyl-2-methylimidazole, 1-benzyl-2-ethylimidazole, 2-phenylimidazole, 2-dodecylimidazole, 1-cyanoethyl substituted imidazole, 1-methylimidazole-phenyl hydroglycerol ether adduct, 2-ethyl-4-methylimidazole carboxylate, 2-methylimidazolyl-1-ethylurea or bis(2-methylimidazolyl-1-ethyl)urea.

[0041] Furthermore, the hydrazide accelerator includes but is not limited to any one of succinic acid hydrazide, adipic acid dihydrazide, sebacic acid dihydrazide or isophthalic acid hydrazide, or a combination of at least two thereof.

[0042] Preferably, the filler includes a first filler and a second filler;

[0043] Among the above fillers, the particle size of the first filler is ≤12μm, for example, it can be 12μm, 11μm, 10μm, 9μm, 8μm, 7μm, 6μm, 5μm, 4μm, 3μm, 2μm, 1μm, etc. The particle size of the second filler is ≤15μm, for example, it can be 15μm, 14μm, 13μm, 12μm, 11μm, 10μm, 9μm, 8μm, 7μm, 6μm, 5μm, 4μm, 3μm, 2μm, 1μm, etc.

[0044] Preferably, the mass ratio of the first filler to the second filler is (10-20):(1-15);

[0045] Among them, "10-20" can be, for example, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, etc.; "1-15" can be, for example, 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, etc.

[0046] Furthermore, in the raw materials for preparing the packaging ink, the content of the first filler is 10 to 20 parts, for example, it can be 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, etc.

[0047] Furthermore, in the raw materials for preparing the packaging ink, the content of the second filler is 1 to 15 parts, for example, it can be 1 part, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, 9 parts, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, etc.

[0048] Preferably, the first filler is selected from any one or a combination of at least two of barium sulfate, talc, mica powder, calcium carbonate or silicon dioxide, preferably silicon dioxide.

[0049] Preferably, the second filler is selected from any one or a combination of at least two of barium sulfate, talc, mica powder, calcium carbonate or silicon dioxide, preferably mica powder.

[0050] It should be noted that the first filler of the present invention is selected from silicon dioxide, and the second filler is selected from mica powder. The toughness of mica powder can improve the brittleness caused by using silicon dioxide alone, and silicon dioxide can also provide film hardness.

[0051] Preferably, the raw materials for preparing the packaging ink further include 1 to 8 parts of an auxiliary agent, for example, 1 part, 2 parts, 3 parts, 4 parts, 5 parts, 6 parts, 7 parts, 8 parts, etc.

[0052] Preferably, the auxiliary agent is selected from any one or a combination of at least two of a defoaming agent, a leveling agent, a film-forming auxiliary agent, a thickener or a wetting and dispersing agent.

[0053] Furthermore, the defoaming agent is selected from any one or a combination of at least two of polyether defoaming agents, silicone defoaming agents or mineral oil defoaming agents; for example, it can be BYK-1790, KS66, BYK-052n, BYK-066n, etc.

[0054] Furthermore, the leveling agent is selected from silicone leveling agents and / or non-silicone leveling agents; for example, it can be 233A.

[0055] Furthermore, the film-forming aid is selected from alcohol ether film-forming aids and / or divalent acid ester film-forming aids; for example, it can be BDG.

[0056] Furthermore, the thickener is selected from mica powder and / or fumed silica.

[0057] Furthermore, the wetting and dispersing agent is selected from any one or a combination of at least two of polyether wetting and dispersing agents, polycarboxylate wetting and dispersing agents, phosphate wetting and dispersing agents, carboxylate wetting and dispersing agents or non-ionic polyethylene oxide block copolymer dispersants; for example, it can be P-193, 680U.

[0058] Preferably, the raw materials for preparing the packaging ink further include 4 to 8 parts of pigment, for example, 4 parts, 4.5 parts, 5 parts, 5.5 parts, 6 parts, 6.5 parts, 7 parts, 7.5 parts, 8 parts, etc.

[0059] Preferably, the raw materials for preparing the packaging ink also include 10 to 20 parts of a solvent, for example, 10 parts, 11 parts, 12 parts, 13 parts, 14 parts, 15 parts, 16 parts, 17 parts, 18 parts, 19 parts, 20 parts, etc.

[0060] Preferably, the solvent is selected from any one of ether solvents, ester solvents, alcohol solvents or ketone solvents, or a combination of at least two thereof.

[0061] Furthermore, the ether solvent is selected from any one of methyl ether, ethyl ether, methyl tert-butyl ether, ethylene glycol dimethyl ether, diethylene glycol dimethyl ether, tetraethylene glycol dimethyl ether, petroleum ether or diethylene glycol monobutyl ether, or a combination of at least two thereof.

[0062] Furthermore, the ester solvent is selected from any one of dimethyl succinate, dimethyl glutarate or dimethyl adipate, or a combination of at least two thereof.

[0063] Furthermore, the alcohol solvent is selected from any one of methanol, ethanol, n-propanol or isopropanol, or a combination of at least two thereof.

[0064] Furthermore, the ketone solvent is selected from any one of acetone, butanone, methyl isobutyl ketone, cyclohexanone, 2-butanone or cyclopropanone, or a combination of at least two thereof.

[0065] In a preferred embodiment of the present invention, the solvent is a dibasic acid ester, also known as DBE, whose main components are dimethyl succinate, dimethyl glutarate, and dimethyl adipate. DBE is notable for its mild odor and low vapor pressure. Its high boiling point and strong dissolving power contribute to a uniform volatilization rate throughout the coating drying process, which helps achieve excellent leveling and gloss, while eliminating surface defects such as fogging, pinholes, and shrinkage cavities.

[0066] In a second aspect, the present invention provides a method for preparing the packaging ink according to the first aspect, the preparation method comprising the following steps:

[0067] The raw materials for preparing the packaging ink are mixed, and then stirred, dispersed, ground, and filtered in sequence to obtain the packaging ink.

[0068] Preferably, the stirring and dispersing speed is 300-500 rpm, for example, it can be 300 rpm, 320 rpm, 340 rpm, 360 rpm, 380 rpm, 400 rpm, 420 rpm, 440 rpm, 460 rpm, 480 rpm, 500 rpm, etc., and the stirring and dispersing time is 1-1.5 h, for example, it can be 1 h, 1.1 h, 1.2 h, 1.3 h, 1.4 h, 1.5 h, etc.

[0069] Preferably, the grinding is performed by using a three-roll grinding slurry for 1 to 5 times, for example, 1 time, 2 times, 3 times, 4 times, 5 times, etc.

[0070] Preferably, the mesh size of the filtration is 200 to 400 meshes.

[0071] Preferably, the viscosity of the packaging ink is 35,000 to 45,000 cP, for example, 35,000 cP, 36,000 cP, 37,000 cP, 38,000 cP, 39,000 cP, 40,000 cP, 41,000 cP, 42,000 cP, 43,000 cP, 44,000 cP, 45,000 cP, etc.

[0072] In the present invention, the method for preparing the packaging ink further includes the step of preparing a first epoxy resin:

[0073] The organic silicon type epoxy resin and the core-shell structure phenolic epoxy prepolymer are mixed and blended and dispersed to obtain a blend, namely the first epoxy resin.

[0074] Preferably, the rotation speed of the blending and dispersion is 400-600 rpm, for example, it can be 400 rpm, 420 rpm, 440 rpm, 460 rpm, 480 rpm, 500 rpm, 520 rpm, 540 rpm, 560 rpm, 580 rpm, 600 rpm, etc., and the blending and dispersion time is 10-30 min, for example, it can be 10 min, 12 min, 14 min, 16 min, 18 min, 20 min, 22 min, 24 min, 26 min, 28 min, 30 min, etc.

[0075] As a preferred technical solution of the present invention, the packaging ink is prepared by the following steps:

[0076] S1, mixing the organosilicon epoxy resin and the core-shell structure phenolic epoxy prepolymer, stirring and dispersing them at a speed of 400 to 600 rpm for 10 to 30 minutes to obtain a first epoxy resin;

[0077] S2. After mixing the first epoxy resin, the second epoxy resin, the curing agent, the curing accelerator, the first filler, the second filler, the auxiliary agent, the pigment and the solvent, the mixture is stirred and dispersed at a speed of 300 to 500 rpm for 1 to 1.5 hours, and then ground by three-roll grinding and filtered to obtain the encapsulation ink.

[0078] In a third aspect, the present invention provides a use of the packaging ink as described in the first aspect in semiconductor passive component packaging.

[0079] In a fourth aspect, the present invention provides a semiconductor device comprising a stack formed of the encapsulation ink according to the first aspect.

[0080] The deposited body is a structure formed after the ink is fixed.

[0081] In a fifth aspect, the present invention provides a device comprising a deposited body formed by the encapsulation ink according to the first aspect, or the semiconductor device according to the fourth aspect.

[0082] The device may be at least a packaged semiconductor device connected to a circuit or cable, etc., and may be capable of achieving a basic function.

[0083] Compared with the prior art, the present invention has the following beneficial effects:

[0084] The packaging ink of the present invention significantly improves the ink's resistance to cold and hot shocks, water resistance, and resistance to folding and cracking by optimizing its composition and ratio, including mixing a first epoxy resin, a second epoxy resin, a curing agent, a curing agent accelerator, a first filler, a second filler, an additive, a pigment, and a solvent, thereby achieving more excellent application performance. DETAILED DESCRIPTION

[0085] Unless otherwise defined herein, scientific and technical terms used in conjunction with the present invention shall have the meanings commonly understood by those of ordinary skill in the art. The meaning and scope of the terms should be clear; however, in the event of any potential ambiguity, the definitions provided herein take precedence over any dictionary or external definitions. In this application, the use of "or" means "and / or" unless otherwise stated. In addition, the use of the term "including" and other forms is non-limiting.

[0086] It should be noted that the following description sets forth specific details to facilitate a full understanding of the present invention. However, the present invention can be implemented in a variety of other ways than those described herein, and those skilled in the art may make similar generalizations without departing from the scope of the present invention. Therefore, the present invention is not limited to the specific embodiments disclosed below.

[0087] The following will clearly and completely describe the technical solutions of the present invention in conjunction with the embodiments. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention.

[0088] The present invention is further described below by way of examples. Unless otherwise specified, the materials in the examples were prepared according to existing methods or directly purchased from the market.

[0089] The sources of the components in the following examples and comparative examples are as follows:

[0090]

[0091]

[0092] Example 1

[0093] This embodiment provides an ink for packaging. The raw materials for preparing the ink for packaging include the following components in parts by weight:

[0094]

[0095] The packaging ink is prepared by the following steps:

[0096] S1, mixing the organosilicon epoxy resin and the core-shell phenolic epoxy prepolymer, stirring and dispersing them at a speed of 500 rpm for 20 minutes to obtain a first epoxy resin;

[0097] S2. After mixing the first epoxy resin, the second epoxy resin, the curing agent, the curing accelerator, the first filler, the second filler, the auxiliary agent, the pigment and the solvent, the mixture was stirred and dispersed at a speed of 500 rpm for 1.2 hours, and then ground twice with a three-roll grinder. Then, the mixture was placed in a three-roll grinder and ground twice, and then filtered at 60° C. using a filter to obtain the encapsulation ink.

[0098] Example 2

[0099] This embodiment provides an ink for packaging. The raw materials for preparing the ink for packaging include the following components in parts by weight:

[0100]

[0101] The preparation method of the packaging ink is consistent with that of Example 1.

[0102] Example 3

[0103] This embodiment provides an ink for packaging. The raw materials for preparing the ink for packaging include the following components in parts by weight:

[0104]

[0105]

[0106] The preparation method of the packaging ink is consistent with that of Example 1.

[0107] Example 4

[0108] This embodiment provides an ink for packaging. The raw materials for preparing the ink for packaging include the following components in parts by weight:

[0109]

[0110] The preparation method of the packaging ink is consistent with that of Example 1.

[0111] Example 5

[0112] This embodiment provides an ink for packaging. The raw materials for preparing the ink for packaging include the following components in parts by weight:

[0113]

[0114]

[0115] The preparation method of the packaging ink is consistent with that of Example 1.

[0116] Example 6

[0117] This embodiment provides an ink for packaging. The raw materials for preparing the ink for packaging include the following components in parts by weight:

[0118]

[0119] The preparation method of the packaging ink is consistent with that of Example 1.

[0120] Example 7

[0121] This embodiment provides an ink for packaging. The raw materials for preparing the ink for packaging include the following components in parts by weight:

[0122]

[0123]

[0124] The preparation method of the packaging ink is consistent with that of Example 1.

[0125] Example 8

[0126] This embodiment provides an ink for packaging, which differs from Example 1 only in that 15 parts of silicon dioxide are replaced with 15 parts of barium sulfate, and the contents of other components and the preparation method are the same as those in Example 1.

[0127] Example 9

[0128] This embodiment provides an ink for packaging, which differs from Example 1 only in that 9 parts of mica powder are replaced with 9 parts of talc powder, and the contents of other components and the preparation method are the same as those in Example 1.

[0129] Example 10

[0130] This embodiment provides an ink for packaging, which differs from Example 1 only in that the content of silicon dioxide is reduced to 9 parts and the content of mica powder is increased to 15 parts. The contents of other components and the preparation method are the same as those in Example 1.

[0131] Comparative Example 1

[0132] This comparative example provides an ink for packaging, and the raw materials for preparing the ink for packaging include the following components in parts by weight:

[0133]

[0134]

[0135] The preparation method of the packaging ink is consistent with that of Example 1.

[0136] Comparative Example 2

[0137] This comparative example provides an ink for packaging, and the raw materials for preparing the ink for packaging include the following components in parts by weight:

[0138]

[0139] The preparation method of the packaging ink is consistent with that of Example 1.

[0140] Comparative Example 3

[0141] This comparative example provides an ink for packaging, and the raw materials for preparing the ink for packaging include the following components in parts by weight:

[0142]

[0143]

[0144] The preparation method of the packaging ink is consistent with that of Example 1.

[0145] Comparative Example 4

[0146] This comparative example provides an ink for packaging, and the raw materials for preparing the ink for packaging include the following components in parts by weight:

[0147]

[0148] The preparation method of the packaging ink is consistent with that of Example 1.

[0149] Comparative Example 5

[0150] This comparative example provides an ink for packaging, and the raw materials for preparing the ink for packaging include the following components in parts by weight:

[0151]

[0152] The preparation method of the packaging ink is consistent with that of Example 1.

[0153] Comparative Example 6

[0154] This comparative example provides an ink for packaging, and the raw materials for preparing the ink for packaging include the following components in parts by weight:

[0155]

[0156]

[0157] The preparation method of the packaging ink is consistent with that of Example 1.

[0158] Comparative Example 7

[0159] This comparative example provides an ink for packaging, and the raw materials for preparing the ink for packaging include the following components in parts by weight:

[0160]

[0161] The preparation method of the packaging ink is consistent with that of Example 1.

[0162] Comparative Example 8

[0163] This comparative example provides an ink for packaging, which differs from Example 1 in that the silicone-based epoxy resin is replaced with an equal mass of naphthalene-based epoxy resin, and the contents of other components and the preparation method are consistent with those of Example 1.

[0164] Comparative Example 9

[0165] This comparative example provides an ink for packaging, which differs from Example 1 in that the silicone epoxy resin is replaced with an acrylic epoxy resin of equal mass, and the contents of other components and the preparation method are consistent with those of Example 1.

[0166] Performance Testing

[0167] Test samples: packaging inks provided in Examples 1 to 10, and packaging inks provided in Comparative Examples 1 to 9;

[0168] Test method:

[0169] During testing, the ink is applied to the substrate surface by screen printing, inkjet printing, gravure printing, spin coating, spray coating, roller coating, or doctor blade coating. Finally, the ink is cured at a temperature range of 120-250°C for 30 minutes to obtain a dense and smooth ink coating with a thickness of 10-30 μm, with a curing temperature range of 150-230°C being preferred.

[0170] Here, a 325-mesh screen was used to screen-print insulating ink for passive component packaging. The ink was then heated in a hot air circulation drying oven at 200°C for 30 minutes to form a 15μm thick insulating ink coating (with an error of ±3μm). The following tests were then performed:

[0171] (1) Viscosity test

[0172] The viscosity of the ink at 25°C was measured using a DV2THBTJ0 viscometer with a 14# rotor and a rotation speed of 100 r / min.

[0173] The viscosity evaluation criteria are as follows:

[0174] ○: viscosity is within the range of 35000 to 45000 cP;

[0175] ×: The viscosity is not within the range of 35,000 to 45,000 cP.

[0176] (2) Film thickness uniformity test

[0177] A 0.85 × 60 mm pattern was printed on a 70 × 60 mm blank ceramic substrate with grooves using a 325 mesh stainless steel screen. After curing at 200°C for 30 min, 12 sample points covering the entire substrate were tested, including the top, bottom, left, right, and center.

[0178] The evaluation criteria for film thickness uniformity test are as follows:

[0179] ○: The extreme difference of film thickness at 12 sample points is ≤ 2 μm;

[0180] ×: The extreme difference in film thickness at 12 sample points is greater than 2 μm.

[0181] (3) Acid resistance test

[0182] A 2×2mm×100-piece silk screen was used to print a pattern with a thickness of 15±3 on a blank substrate without grooves. Two samples were sampled after the pattern was cured and immersed in 5 parts hydrochloric acid and 5 parts sulfuric acid solutions for 1 hour respectively. The surface was cleaned with deionized water, dried, and the appearance was observed. The samples were then torn vertically with 3M tape.

[0183] The acid resistance test evaluation criteria are as follows:

[0184] ○: There is no corrosion on the graphic appearance after acid immersion, and the 3M tape does not fall off when torn vertically;

[0185] ×: The graphics are corroded after acid immersion, and the 3M tape falls off when torn vertically.

[0186] (4) Solvent resistance test

[0187] A 2×2mm×100-piece silk screen was used to print a pattern with a thickness of 15±3 on a blank substrate without grooves. Two samples were sampled after the pattern was cured and immersed in a solution of isopropyl alcohol: butanone = 1:1 for 1 hour. The surface was cleaned with deionized water, dried, and observed for appearance. The samples were then torn vertically with 3M tape.

[0188] The evaluation criteria for solvent resistance testing are as follows:

[0189] ○: There is no corrosion on the graphic appearance after solvent immersion, and the 3M tape does not fall off when torn vertically;

[0190] ×: The graphics are corroded after being soaked in solvent, and the 3M tape falls off when torn vertically.

[0191] (5) Anti-fragmentation and cracking test:

[0192] A 0.85×60 mm pattern was printed on a 70×60 mm blank ceramic substrate with grooves using a 325-mesh stainless steel screen. After curing at 200°C for 30 minutes, the pattern was folded using a 0201 folding machine.

[0193] The evaluation criteria for folding and breaking properties are as follows:

[0194] ○: ink coating damage rate <5 parts;

[0195] ×: The ink coating damage rate is ≥5 copies.

[0196] (6) Adhesion test:

[0197] Use a silk screen with a graphic design of 2×2mm×100pcs to print a pattern with a thickness of 15±3μm on a blank substrate without grooves. After sampling one piece of the pattern and curing, the sample is boiled in water at normal pressure for 16h (the time can be accumulated) and then dried, and then vertically torn using 3M tape.

[0198] The adhesion test evaluation criteria are as follows:

[0199] ○: 3M tape does not fall off when torn vertically;

[0200] ×: The 3M tape falls off when torn vertically.

[0201] (7) Heat resistance test:

[0202] A 50mm×50mm pattern with a thickness of 15μm (error ±3μm) was printed on a blank ceramic substrate. After curing at 200℃ for 30min, the pattern was immersed in a tin furnace at 288℃ for 10s / 3 times.

[0203] The heat resistance test evaluation criteria are as follows:

[0204] ○: The ink coating is intact and has no cracks;

[0205] ×: The ink coating is peeled or cracked.

[0206] The specific test results are shown in Table 1:

[0207] Table 1

[0208]

[0209]

[0210] The above results show that the viscosity of the packaging ink of the present invention is 35000~45000 cP; in the film thickness uniformity test, the thickness range of 12 samples that can cover the entire substrate is ≤2μm; in the acid resistance test, after being immersed in a strong acid mixture of hydrochloric acid and sulfuric acid for 1 hour, the appearance of the graphics is not corroded, and there is no falling off even when 3M tape is used to tear it vertically; in the solvent resistance test, after being immersed in an organic mixture of isopropyl alcohol and butanone for 1 hour, the appearance of the graphics is not corroded, and there is no falling off even when 3M tape is used to tear it vertically There is no falling off phenomenon even when being torn; in the test of resistance to folding and cracking, the ink coating breakage rate is less than 5 parts when folded by a folding machine; in the adhesion test, there is no falling off phenomenon after boiling in water at normal pressure for 16 hours and then tearing vertically with 3M tape; in the heat resistance test, the ink coating is intact and has no cracks after being immersed in a tin furnace at 288°C for 10s / 3 times; it can be fully said that the ink for semiconductor passive component packaging provided by the present invention has the characteristics of good acid resistance, solvent resistance, resistance to folding and cracking, excellent adhesion and heat resistance.

[0211] Among them, comparing Examples 1 to 3 with Comparative Examples 1 to 3, it can be seen that the addition of silicone epoxy resin and core-shell phenolic epoxy prepolymer in the amounts described above resulted in all test results passing. However, Comparative Example 1, which did not add silicone epoxy resin, failed the acid resistance, solvent resistance, adhesion, and heat resistance tests. Comparative Example 2, which did not add core-shell phenolic epoxy prepolymer, failed the folding and cracking test. In Comparative Example 3, insufficient addition of silicone epoxy resin and core-shell phenolic epoxy prepolymer resulted in the ink coating failing the acid resistance, solvent resistance, folding and cracking test, adhesion, and heat resistance tests.

[0212] Among them, Examples 4 to 7 are compared with Comparative Examples 4 to 7. It can be seen that the addition of silicone epoxy resin and core-shell phenolic epoxy prepolymer and the addition amount within the range can improve the acid resistance, solvent resistance, particle breakage, adhesion and heat resistance of the ink coating. Too little or too much will be detrimental to the acid resistance, solvent resistance, particle breakage, adhesion and heat resistance of the ink coating.

[0213] Among them, in Comparative Examples 4 and 7, too little core-shell phenolic epoxy prepolymer was added. Although the ink coating passed the acid resistance, solvent resistance, and particle folding cracking test, it failed the particle folding cracking test. In Comparative Example 7, excessive addition of silicone epoxy resin resulted in excessive viscosity and failed the test.

[0214] Among them, in Comparative Examples 5 and 6, too little silicone epoxy resin was added, and the ink failed the acid resistance, solvent resistance, adhesion, and heat resistance tests. In Comparative Example 6, too much silicone epoxy resin was added, resulting in excessive viscosity and failure.

[0215] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, rather than to limit it. Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art should understand that they can still modify the technical solutions described in the above embodiments, or replace some or all of the technical features therein with equivalents. However, these modifications or replacements do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A packaging ink, characterized in that: The raw materials for preparing the packaging ink include the following components in parts by weight: 20-35 parts of the first epoxy resin, 1-10 parts of the second epoxy resin, 3-7 parts of the curing agent, 0.15-7 parts of the curing accelerator, and 10-35 parts of the filler; Wherein, the first epoxy resin comprises an organosilicon epoxy resin and a core-shell structure phenolic epoxy prepolymer; Wherein, the second epoxy resin includes novolac epoxy resin.

2. The packaging ink according to claim 1, characterized in that The mass ratio of the silicone epoxy resin to the core-shell structure novolac epoxy prepolymer is (1-2.5):(1-2.5).

3. The packaging ink according to claim 1, wherein The epoxy equivalent of the silicone epoxy resin is 230-250 g / eq.

4. The packaging ink according to claim 1, wherein The content of rubber in the core-shell structure phenolic epoxy prepolymer is 30-45 wt%.

5. The packaging ink according to claim 1, wherein The epoxy equivalent of the core-shell structured novolac epoxy prepolymer is 260-280 g / eq.

6. The packaging ink according to claim 1, wherein The epoxy equivalent of the novolac epoxy resin is 185-195 g / eq.

7. The encapsulation ink according to claim 1, wherein The molecular weight of the novolac epoxy resin is 500-700 g / mol.

8. The encapsulation ink according to claim 1, wherein The total chlorine content of the novolac epoxy resin is ≤1200 ppm.

9. The packaging ink according to claim 1, wherein The melting temperature of the novolac epoxy resin is less than 90°C.

10. The packaging ink according to claim 1, characterized in that The curing agent is a latent amine curing agent containing active hydrogen.

11. The packaging ink according to claim 10, characterized in that The amine value of the curing agent is ≥50, and the active hydrogen equivalent is 140-145.

12. The packaging ink according to claim 10, characterized in that The latent amine curing agent is selected from any one of dicyandiamide, diaminodiphenyl sulfone or adipic acid dihydrazide, or a combination of at least two thereof.

13. The packaging ink according to claim 1, wherein The curing accelerator is selected from any one of urea accelerators, phenol accelerators, imidazole accelerators or hydrazide accelerators, or a combination of at least two thereof.

14. The packaging ink according to claim 1, wherein The filler includes a first filler and a second filler; Wherein, the particle size of the first filler is ≤12 μm, and the particle size of the second filler is ≤15 μm.

15. The packaging ink according to claim 14, characterized in that The mass ratio of the first filler to the second filler is (10-20):(1-15).

16. The packaging ink according to claim 14, characterized in that The first filler is selected from any one of barium sulfate, talc powder, mica powder, calcium carbonate or silicon dioxide, or a combination of at least two thereof.

17. The packaging ink according to claim 16, characterized in that The first filler is silicon dioxide.

18. The packaging ink according to claim 14, wherein The second filler is selected from any one of barium sulfate, talc, mica powder, calcium carbonate or silicon dioxide, or a combination of at least two thereof.

19. The packaging ink according to claim 18, characterized in that The second filler is mica powder.

20. The packaging ink according to claim 1, characterized in that The raw materials for preparing the packaging ink also include 1 to 8 parts of auxiliary agents.

21. The encapsulation ink according to claim 20, characterized in that The auxiliary agent is selected from any one or a combination of at least two of a defoaming agent, a leveling agent, a film-forming auxiliary agent, a thickener or a wetting and dispersing agent.

22. The packaging ink according to claim 1, characterized in that The raw materials for preparing the packaging ink also include 4 to 8 parts of pigment.

23. The encapsulation ink according to claim 1, characterized in that The raw materials for preparing the packaging ink also include 10 to 20 parts of a solvent.

24. The encapsulation ink according to claim 23, characterized in that The solvent is selected from any one of ether solvents, ester solvents, alcohol solvents or ketone solvents, or a combination of at least two thereof.

25. A method for preparing an encapsulation ink according to any one of claims 1 to 24, characterized in that: The preparation method comprises the following steps: The raw materials for preparing the packaging ink are mixed, and then stirred, dispersed, ground, and filtered in sequence to obtain the packaging ink.

26. The method for preparing the packaging ink according to claim 25, wherein: The stirring and dispersing speed is 300-500 rpm, and the stirring and dispersing time is 1-1.5 h.

27. The method for preparing the packaging ink according to claim 25, wherein: The grinding is performed by using a three-roll grinding slurry for 1 to 5 times.

28. The method for preparing the packaging ink according to claim 25, wherein: The mesh size of the filtration is 200-400 meshes.

29. The method for preparing the packaging ink according to claim 25, wherein: The viscosity of the packaging ink is 35,000 to 45,000 cP.

30. Use of the packaging ink according to any one of claims 1 to 24 in semiconductor passive component packaging.

31. A semiconductor device, characterized in that The semiconductor device includes a deposited body formed of the encapsulation ink according to any one of claims 1 to 24.

32. A device, characterized in that The device includes a deposit formed of the encapsulation ink according to any one of claims 1 to 24, or the semiconductor device according to claim 31.

Citation Information

Patent Citations

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