Thermosetting resin mixed wax for wafer processing and preparation method thereof

Abstract

According to the thermosetting resin mixed wax for wafer processing and the preparation method thereof provided by the invention, the mixed wax is composed of the specific low-acid-value oxidized polyethlene wax and the high-acid-value oxidized polyethlene wax, so that a synergistic effect can be achieved, and the compatibility of thermosetting resin and inorganic filler is improved; and meanwhile, the high-temperature fluidity, the adhesion and the warping resistance of the thermosetting resin composition are considered.

Description

Technical Field

[0001] The invention belongs to the technical field of wafer processing, and in particular relates to a thermosetting resin mixed wax for wafer processing and a preparation method thereof. Background Art

[0002] As the requirements for electronic equipment to be lightweight and miniaturized continue to increase, the requirements for wafer packaging to be thinner and smaller are also increasing. In the prior art, wafer packaging usually uses thermosetting resin as a sealing material for curing and packaging. Common thermosetting resins include epoxy resins, phenolic resins, silicone resins, and silicone resins. In order to meet the requirements of thinness and miniaturization, the curing process of the above thermosetting resins is prone to warping. Adding inorganic fillers can improve the warping phenomenon, but it is easy to cause the thermosetting resin composition to have an increased melt viscosity, reduced flexibility, and poor processability, and even cause shedding and cracking problems. Summary of the invention

[0003] In order to overcome the problems existing in the prior art, the purpose of the present invention is to provide a thermosetting resin mixed wax for wafer processing and a preparation method thereof, which adopts a specific low-acid value oxidized polyethylene wax and a high-acid value oxidized polyethylene wax to form a mixed wax, which can play a synergistic role, improve the compatibility of the thermosetting resin and the inorganic filler, and at the same time take into account the high-temperature fluidity, adhesion and warping resistance of the thermosetting resin composition.

[0004] The objective of the present invention is achieved through the following technical solutions:

[0005] A thermosetting resin mixed wax for wafer processing comprises 80-120 parts of thermosetting resin, 15-45 parts of modified filler, 5-25 parts of mixed wax and 3-15 parts of MBS toughening agent; the modified filler is an inorganic filler modified by a silane coupling agent, and the silane coupling agent is an epoxy silane coupling agent; the mixed wax consists of a low acid value oxidized polyethylene wax and a high acid value oxidized polyethylene wax in a mass ratio of 2-4:1.

[0006] Preferably, the acid value of the low acid value oxidized polyethylene wax is 1.0-20.0, and the acid value of the high acid value oxidized polyethylene wax is 30.0-80.0.

[0007] Preferably, the acid value of the low acid value oxidized polyethylene wax is 1.0-15.0, and the acid value of the high acid value oxidized polyethylene wax is 40.0-80.0.

[0008] Preferably, the acid value of the low acid value oxidized polyethylene wax is 1.0-12.0, and the acid value of the high acid value oxidized polyethylene wax is 40.0-60.0.

[0009] Preferably, the mixed wax consists of low acid value oxidized polyethylene wax and high acid value oxidized polyethylene wax in a mass ratio of 2-3:1.

[0010] Preferably, the thermosetting resin is one or more of phenolic resin, epoxy resin, silicone resin and polyester resin.

[0011] Preferably, the thermosetting resin is an epoxy resin, and its preparation raw materials include bisphenol A epoxy resin and a curing accelerator, or biphenyl epoxy resin and a curing accelerator.

[0012] Preferably, the thermosetting resin is a silicone resin, and its preparation raw materials include component A and component B, wherein component A includes, by weight: 30-60 parts of end-side vinyl polysiloxane and 0.2-0.5 parts of platinum catalyst; component B includes, by weight: 20-50 parts of end-side vinyl polysiloxane and 10-30 parts of end-side hydrogen-containing polysiloxane.

[0013] Preferably, the inorganic filler is one or more of carbon fiber, glass fiber, silica, mica, talc, alumina, silicon carbide, calcium carbonate, and barium titanate.

[0014] Preferably, the silane coupling agent is KH560.

[0015] A method for preparing a thermosetting resin mixed wax for wafer processing comprises the following reaction steps:

[0016] Step 1: Mix the epoxy silane coupling agent modified filler with the high acid value oxidized polyethylene wax, heat and stir to disperse at 80-150° C. for 1-3 hours, and cool to room temperature after stirring to obtain a pretreated modified filler;

[0017] Step 2: weigh the raw materials for preparing thermosetting resin, add the pretreated modified filler, low acid value oxidized polyethylene wax and MBS toughening agent, stir and mix, and prepare the thermosetting resin mixed wax for wafer processing.

[0018] Preferably, a method for preparing a thermosetting resin mixed wax for wafer processing comprises the following reaction steps:

[0019] Step 1: Mix the epoxy silane coupling agent modified filler with the high acid value oxidized polyethylene wax, heat and stir to disperse at 80-150° C. for 1-3 hours, and cool to room temperature after stirring to obtain a pretreated modified filler;

[0020] Step 2, weighing component A and component B for preparing thermosetting resin raw materials, stirring and mixing component A raw materials and pre-treated modified fillers to obtain mixture A, stirring and mixing component B with low acid value oxidized polyethylene wax and MBS toughening agent to obtain mixture B;

[0021] Step three, stirring and mixing the mixture A and the mixture B to obtain a thermosetting resin mixed wax for wafer processing.

[0022] Beneficial effects:

[0023] 1. The mixed wax composed of specific low acid value oxidized polyethylene wax and high acid value oxidized polyethylene wax can play a synergistic role to improve the compatibility of thermosetting resin and inorganic filler, while taking into account the high temperature fluidity, adhesion and warpage resistance of the thermosetting resin composition.

[0024] 2. Use epoxy silane coupling agent to modify the inorganic filler, introduce epoxy groups, and form chemical bonds through ring-opening reaction with hydroxyl groups in oxidized polyethylene wax to modify the surface of the inorganic filler, improve the compatibility of the inorganic filler with thermosetting resin, and improve the high-temperature fluidity, adhesion and warping resistance of the thermosetting resin composition.

[0025] 3. Use high acid value oxidized polyethylene wax to coat and modify the epoxy silane coupling agent modified inorganic filler for pretreatment, and then add it to the thermosetting resin raw material with low acid value oxidized polyethylene wax. This can not only make the high acid value oxidized polyethylene wax more fully and stably coat and modify the inorganic filler, fix it to the surface of the inorganic filler through chemical bonds, and improve the high temperature fluidity and warping resistance of the thermosetting resin composition, but also use the low acid value oxidized polyethylene wax to exert better adhesion and demolding properties. DETAILED DESCRIPTION

[0026] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are part of the embodiments of the present invention, rather than all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0027] The present invention is further explained below in conjunction with specific implementation modes.

[0028] Example 1

[0029] A thermosetting resin mixed wax for wafer processing, comprising a thermosetting resin, 35 parts of KH560 modified carbon fiber, 12 parts of mixed wax, and 5 parts of MBS toughening agent; the mixed wax is composed of a low acid value oxidized polyethylene wax and a high acid value oxidized polyethylene wax in a mass ratio of 2:1, the low acid value oxidized polyethylene wax is HI-Wax 4051E, the acid value is 12, and the high acid value oxidized polyethylene wax is HI-Wax 1105A, the acid value is 60. The thermosetting resin is an organic silicone resin, and its preparation raw materials include component A and component B, wherein component A includes, by weight, 50 parts of end-side vinyl polysiloxane and 0.5 parts of platinum catalyst; component B includes, by weight, 30 parts of end-side vinyl polysiloxane and 20 parts of end-side hydrogen-containing polysiloxane. The end-side vinyl polysiloxane is ELASTOSIL LR3003, and the end-side hydrogen-containing polysiloxane is ELASTOSIL LR3011.

[0030] The preparation method thereof comprises the following reaction steps:

[0031] Step 1: Mix the KH560 modified carbon fiber and the high acid value oxidized polyethylene wax HI-Wax 1105A, heat and stir to disperse at 120° C. for 1 hour, and cool to room temperature after stirring to obtain a pretreated modified filler;

[0032] Step 2, weighing component A and component B for preparing thermosetting resin raw materials, stirring and mixing component A raw materials and pre-treated modified fillers to obtain mixture A, stirring and mixing component B with low acid value oxidized polyethylene wax HI-Wax 4051E and MBS toughening agent to obtain mixture B;

[0033] Step three, stirring and mixing the mixture A and the mixture B to obtain a thermosetting resin mixed wax, applying the mixed wax to the back of the wafer, and curing it at 180° C. for 1 hour to obtain a back adhesive layer with a thickness of 1 mm.

[0034] Comparative Example 1

[0035] A thermosetting resin mixed wax for wafer processing is prepared according to the method of Example 1, the only difference being that the modified filler KH560 modified carbon fiber is replaced by KH570 modified carbon fiber.

[0036] Comparative Example 2

[0037] A thermosetting resin mixed wax for wafer processing is prepared according to the method of Example 1, the only difference being that the low acid value oxidized polyethylene wax and the high acid value oxidized polyethylene wax are added in a different order. The preparation method comprises the following reaction steps:

[0038] Step 1: Mix the KH560 modified carbon fiber and the low acid value oxidized polyethylene wax HI-Wax 4051E, heat and stir to disperse at 120° C. for 1 hour, and cool to room temperature after stirring to obtain a pretreated modified filler;

[0039] Step 2, weighing component A and component B for preparing thermosetting resin raw materials, stirring and mixing component A raw materials and pre-treated modified fillers to obtain mixture A, stirring and mixing component B with high acid value oxidized polyethylene wax HI-Wax 1105A and MBS toughening agent to obtain mixture B;

[0040] Step three, stirring and mixing the mixture A and the mixture B to obtain a thermosetting resin mixed wax, applying the mixed wax to the back of the wafer, and curing it at 180° C. for 1 hour to obtain a back adhesive layer with a thickness of 1 mm.

[0041] Comparative Example 3

[0042] A thermosetting resin mixed wax for wafer processing is prepared according to the method of Example 1, the only difference being that the low acid value oxidized polyethylene wax and the high acid value oxidized polyethylene wax are added in a different order. The preparation method comprises the following reaction steps:

[0043] Step 1: Mix the KH560 modified carbon fiber with low acid value oxidized polyethylene wax HI-Wax 4051E and high acid value oxidized polyethylene wax HI-Wax 1105A, heat and stir to disperse at 120° C. for 1 hour, and cool to room temperature after stirring to obtain a pretreated modified filler;

[0044] Step 2, weighing component A and component B for preparing thermosetting resin raw materials, stirring and mixing component A raw materials and pre-treated modified fillers to obtain mixture A, and stirring and mixing component B and MBS toughening agent to obtain mixture B;

[0045] Step three, stirring and mixing the mixture A and the mixture B to obtain a thermosetting resin mixed wax, applying the mixed wax to the back of the wafer, and curing it at 180° C. for 1 hour to obtain a back adhesive layer with a thickness of 1 mm.

[0046] Comparative Example 4

[0047] A thermosetting resin mixed wax for wafer processing is prepared according to the method of Example 1, the only difference being that the low acid value oxidized polyethylene wax and the high acid value oxidized polyethylene wax are added in a different order. The preparation method comprises the following reaction steps:

[0048] Step 1, weighing component A and component B for preparing thermosetting resin raw materials, stirring and mixing component A raw materials, KH560 modified carbon fiber and high acid value oxidized polyethylene wax HI-Wax 1105A to obtain mixture A, stirring and mixing component B, low acid value oxidized polyethylene wax HI-Wax 4051E and MBS toughening agent to obtain mixture B;

[0049] Step 2: Stir and mix the mixture A and the mixture B to obtain a thermosetting resin mixed wax, apply the mixed wax to the back of the wafer, and cure it at 180° C. for 1 hour to obtain a back adhesive layer with a thickness of 1 mm.

[0050] Comparative Example 5

[0051] A thermosetting resin mixed wax for wafer processing is prepared according to the method of Example 1, the only difference being that the high acid value oxidized polyethylene wax HI-Wax 1105A is replaced by the low acid value oxidized polyethylene wax HI-Wax 4051E.

[0052] The preparation method thereof comprises the following reaction steps:

[0053] Step 1: Mix KH560 modified carbon fiber with 8 parts of low acid value oxidized polyethylene wax HI-Wax 4051E, heat and stir to disperse at 120° C. for 1 hour, and cool to room temperature after stirring to obtain a pretreated modified filler;

[0054] Step 2, weighing component A and component B for preparing thermosetting resin raw materials, stirring and mixing the component A raw material and the pretreated modified filler to obtain a mixture A, and stirring and mixing component B with 4 parts of low acid value oxidized polyethylene wax HI-Wax 4051E and MBS toughening agent to obtain a mixture B;

[0055] Step three, stirring and mixing the mixture A and the mixture B to obtain a thermosetting resin mixed wax, applying the mixed wax to the back of the wafer, and curing it at 180° C. for 1 hour to obtain a back adhesive layer with a thickness of 1 mm.

[0056] Comparative Example 6

[0057] A thermosetting resin mixed wax for wafer processing is prepared according to the method of Example 1, the only difference being that the low acid value oxidized polyethylene wax HI-Wax 4051E is replaced by the high acid value oxidized polyethylene wax HI-Wax 1105A.

[0058] The preparation method thereof comprises the following reaction steps:

[0059] Step 1: Mix KH560 modified carbon fiber with 8 parts of high acid value oxidized polyethylene wax HI-Wax 1105A, heat and stir to disperse at 120° C. for 1 hour, and cool to room temperature after stirring to obtain a pretreated modified filler;

[0060] Step 2, weighing component A and component B for preparing thermosetting resin raw materials, stirring and mixing component A raw materials and pre-treated modified fillers to obtain mixture A, stirring and mixing component B and 4 parts of high acid value oxidized polyethylene wax HI-Wax 1105A and MBS toughening agent to obtain mixture B;

[0061] Step three, stirring and mixing the mixture A and the mixture B to obtain a thermosetting resin mixed wax, applying the mixed wax to the back of the wafer, and curing it at 180° C. for 1 hour to obtain a back adhesive layer with a thickness of 1 mm.

[0062] Performance Testing

[0063] The thermosetting resin mixed wax and adhesive layer obtained in Example 1 and Comparative Examples 1-6 were characterized.

[0064] Fluidity: CFT-500 flow tester was used to test the melt viscosity of thermosetting resin mixed wax at a pressure of 25kgf and a temperature of 180°C.

[0065] Adhesion: Test the peel strength of the adhesive layer according to JIS / C6481-1996.

[0066] Warpage: The 1mm thick adhesive layer obtained by curing the back of the wafer at 180°C for 1 hour was cooled to room temperature, peeled off from the wafer, and the warpage was measured with a ruler. The results are shown in Table 1.

[0067] Table 1 Properties of thermosetting resin mixed wax and adhesive layer

[0068]

[0069]

[0070] From the comparison between Example 1 and Comparative Example 1, it can be seen that the thermosetting resin mixed wax and the backing layer prepared in Example 1 of the present application have better effects in terms of melt viscosity, peel strength and warpage. This may be because compared with the vinyl silane coupling agent, the epoxy silane coupling agent is used to modify the inorganic filler, and the epoxy group is introduced. The epoxy group reacts with the hydroxyl group, carboxyl group and other groups in the oxidized polyethylene wax to form a chemical bond, and the inorganic filler is surface-coated and modified, and fixed on the surface of the inorganic filler. The high-acid value oxidized polyethylene wax can more fully and stably coat and modify the inorganic filler, thereby improving the high-temperature fluidity and warpage resistance of the thermosetting resin composition, and the low-acid value oxidized polyethylene wax can also be used to exert better adhesion and demolding properties.

[0071] From the comparison of Example 1, Comparative Example 2, Comparative Example 3, and Comparative Example 4, it can be seen that the thermosetting resin mixed wax and the backing layer prepared in Example 1 of the present application have better effects in terms of melt viscosity, peel strength and warpage. This may be due to the use of epoxy silane coupling agent to modify the inorganic filler, introduce epoxy groups, and form chemical bonds through the ring-opening reaction between the epoxy groups and the hydroxyl groups, carboxyl groups and other groups in the high acid value oxidized polyethylene wax, and then carry out surface coating modification on the inorganic filler, fix it on the surface of the inorganic filler, and then add it to the thermosetting resin raw material with the low acid value oxidized polyethylene wax. This can not only make the high acid value oxidized polyethylene wax more fully and stably coat and modify the inorganic filler, improve the high temperature fluidity and warpage resistance of the thermosetting resin composition, but also can utilize the low acid value oxidized polyethylene wax to exert better adhesion and demolding properties.

[0072] From the comparison of Example 1, Comparative Example 5 and Comparative Example 6, it can be seen that the thermosetting resin mixed wax and the backing layer prepared in Example 1 of the present application have a synergistic effect in terms of melt viscosity, peel strength and warpage. This is because the mixed wax composed of specific low-acid value oxidized polyethylene wax and high-acid value oxidized polyethylene wax can play a synergistic role in improving the compatibility of the thermosetting resin and the inorganic filler, while taking into account the high-temperature fluidity, adhesion and warpage resistance of the thermosetting resin composition.

[0073] The above embodiments are preferred implementation modes of the present invention, but the implementation modes of the present invention are not limited to the above embodiments. Any other changes, modifications, substitutions, combinations, and simplifications that do not deviate from the spirit and principles of the present invention should be equivalent replacement methods and are included in the protection scope of the present invention.

Claims

1. A thermosetting resin mixed wax for wafer processing, characterized in that: The invention comprises 80-120 parts of a thermosetting resin, 15-45 parts of a modified filler, 5-25 parts of a mixed wax and 3-15 parts of an MBS toughening agent; the modified filler is an inorganic filler modified by a silane coupling agent, and the silane coupling agent is an epoxy silane coupling agent; the mixed wax is composed of a low-acid-value oxidized polyethylene wax and a high-acid-value oxidized polyethylene wax in a mass ratio of 2-4:1; the acid value of the low-acid-value oxidized polyethylene wax is 1.0-20.0, and the acid value of the high-acid-value oxidized polyethylene wax is 30.0-80.

0.

2. The thermosetting resin mixed wax for wafer processing according to claim 1, characterized in that: The acid value of the low-acid-value oxidized polyethylene wax is 1.0-15.0, and the acid value of the high-acid-value oxidized polyethylene wax is 40.0-80.

0.

3. The thermosetting resin mixed wax for wafer processing according to claim 1, characterized in that: The acid value of the low-acid-value oxidized polyethylene wax is 1.0-12.0, and the acid value of the high-acid-value oxidized polyethylene wax is 40.0-60.

0.

4. The thermosetting resin mixed wax for wafer processing according to claim 1, characterized in that: The thermosetting resin is one or more of phenolic resin, epoxy resin, silicone resin and polyester resin.

5. The thermosetting resin mixed wax for wafer processing according to claim 1, characterized in that: The thermosetting resin is a silicone resin, and its preparation raw materials include component A and component B, wherein component A includes, by weight: 30-60 parts of end-side vinyl polysiloxane and 0.2-0.5 parts of platinum catalyst; component B includes, by weight: 20-50 parts of end-side vinyl polysiloxane and 10-30 parts of end-side hydrogen-containing polysiloxane.

6. The thermosetting resin mixed wax for wafer processing according to claim 1, characterized in that: The inorganic filler is one or more of carbon fiber, glass fiber, silicon dioxide, mica, talc, aluminum oxide, silicon carbide, calcium carbonate, and barium titanate.

7. The thermosetting resin mixed wax for wafer processing according to claim 6, characterized in that: The silane coupling agent is KH560.

8. A method for preparing the thermosetting resin mixed wax for wafer processing according to any one of claims 1 to 7, comprising the following reaction steps: Step 1: Mix the epoxy silane coupling agent modified filler with the high acid value oxidized polyethylene wax, heat and stir to disperse at 80-150° C. for 1-3 hours, and cool to room temperature after stirring to obtain a pretreated modified filler; Step 2: weigh the raw materials for preparing thermosetting resin, add pretreated modified filler, low acid value oxidized polyethylene wax, and MBS toughening agent, stir and mix, and prepare thermosetting resin mixed wax for wafer processing.

9. A method for preparing the thermosetting resin mixed wax for wafer processing according to any one of claims 1 to 7, comprising the following reaction steps: Step 1: Mix the epoxy silane coupling agent modified filler with the high acid value oxidized polyethylene wax, heat and stir to disperse at 80-150° C. for 1-3 hours, and cool to room temperature after stirring to obtain a pretreated modified filler; Step 2, weighing component A and component B for preparing thermosetting resin raw materials, stirring and mixing component A raw materials and pre-treated modified fillers to obtain mixture A, stirring and mixing component B with low acid value oxidized polyethylene wax and MBS toughening agent to obtain mixture B; Step three, stirring and mixing the mixture A and the mixture B to obtain a thermosetting resin mixed wax for wafer processing.

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