A material based on epoxy resin for ESC dielectric layer of aluminum substrate and preparation method thereof

Abstract

The present invention provides an ESC dielectric layer material, including: 10 to 25 parts by weight of bisphenol F epoxy resin, 5 to 30 parts by weight of modified epoxy resin, 5 to 15 parts by weight of acrylic rubber / epoxy resin composite material, 10 to 20 parts by weight of aluminum oxide, 5 to 25 parts by weight of narrow bandgap semiconductor material, 5 to 25 parts by weight of conductive powder, 1 to 5 parts by weight of silane coupling agent, 20 to 30 parts by weight of curing agent and 1 to 5 parts by weight of accelerator. The present invention combines a specific bisphenol F epoxy resin with a modified epoxy resin, so that the material has low surface resistance, strong adhesion and processability after curing; and combines the selection and proportion of conductive powders, through a reasonable combination of a variety of conductive powders, the material can generate J-R force when powered on, and realize stable adsorption of the target object. The material only needs to be heated and cured after coating to obtain an ESC dielectric layer with high adsorption force and long-lasting adsorption force.

Description

Technical Field

[0001] The invention belongs to the technical field of ESC electrostatic chuck adhesive manufacturing, and relates to an ESC dielectric layer material and a preparation method and application thereof, and an ESC substrate, and in particular to an epoxy resin-based material for an aluminum substrate ESC dielectric layer and a preparation method thereof. Background Art

[0002] Epoxy resin adhesive is a type of adhesive made of epoxy resin base material, curing agent, diluent, accelerator and filler. ESC electrostatic chuck is a general term for ultra-clean thin film carriers and gripping and handling equipment suitable for atmospheric or vacuum environments. The electrostatic adsorption technology it uses is an advantageous technology that replaces traditional mechanical clamping and vacuum adsorption methods and is widely used in semiconductors, panel displays, optics and other fields.

[0003] In the context of the continuous development of domestic semiconductor technology, the semiconductor product module bonding process has become the core link to ensure the overall product shipment yield. Especially as the panel display industry enters a new stage of OLED, the bendability of flexible OLED display panels has brought more development directions for terminal display products. However, in the process of flexible product module bonding, traditional bonding technologies, such as mechanical support, vacuum adsorption and 3D bonding, although they meet the needs to a certain extent, often cause mechanical scratches, adsorption bubbles and surface defects during bonding, which seriously affects the product shipment yield.

[0004] Therefore, electrostatic adsorption technology has begun to be widely used and paid attention to in the field of chip manufacturing. This technology usually uses high-purity ceramic slurry to be integrally sintered in SPS (plasma high temperature sintering technology). Its high-voltage electrostatic dielectric layer uses ceramic powder. After surface polishing, it can meet the strict requirements for surface flatness during wafer manufacturing and transportation (required to be less than 10 microns). Although the existing imported ESC substrates are manufactured using ceramic sintering technology, they can obtain higher adsorption force, but due to its complex manufacturing process, high price and difficult maintenance, this kind of ceramic electrostatic chuck is subject to certain restrictions in practical applications. Domestic scholars and technicians mainly improve the original adsorption performance through the new structural design of the electrostatic chuck and its functional innovation, and there are still very few studies on improving the adsorption performance of the electrostatic chuck. Domestic aluminum substrate ESC usually adopts a structure composed of an aluminum substrate, a high-temperature adhesive connection layer, a PEEK insulating film, a silver electrode and an epoxy adhesive dielectric layer, but due to the insufficient adsorption force of the existing epoxy adhesive and the attenuation of the adsorption force with storage time, it cannot meet the needs of efficient and long-lasting adsorption.

[0005] Therefore, how to find a more suitable ESC dielectric layer material to solve the above-mentioned technical problems existing in the existing technical solutions has become one of the urgent problems to be solved by many front-line researchers in the industry. Summary of the invention

[0006] In view of this, the technical problem to be solved by the present invention is to provide an ESC dielectric layer material and its preparation method, application, an ESC (electrostatic chuck) substrate, in particular, an epoxy resin-based material for an aluminum substrate ESC dielectric layer. The ESC dielectric layer material provided by the present invention has strong adhesion, processability and grindability to Peek film, aluminum plate, silver and other materials. After coating, only heating and curing are required to obtain an ESC dielectric layer with high adsorption force and long-lasting adsorption force; and the preparation process is simple, easy to control, and the conditions are mild, which is more conducive to the promotion and application of industrial large-scale production.

[0007] The present invention provides an ESC dielectric layer material, which comprises, by raw material mass fraction:

[0008] 10-25 parts by weight of bisphenol F epoxy resin;

[0009] 5 to 30 parts by weight of modified epoxy resin;

[0010] 5 to 15 parts by weight of acrylic rubber / epoxy resin composite material;

[0011] 10 to 20 parts by weight of aluminum oxide;

[0012] 5 to 25 parts by weight of narrow bandgap semiconductor material;

[0013] 5 to 25 parts by weight of conductive powder;

[0014] 1 to 5 parts by weight of silane coupling agent;

[0015] 20 to 30 parts by weight of curing agent;

[0016] Accelerator 1 to 5 parts by weight.

[0017] Preferably, the ESC dielectric layer material is a material used for the ESC dielectric layer of an aluminum substrate;

[0018] The modified epoxy resin is boron novolac epoxy resin and / or bisphenol A pentyl novolac epoxy resin;

[0019] The acrylic rubber / epoxy resin composite material is acrylic rubber particles dispersed in epoxy resin.

[0020] Preferably, the narrow bandgap semiconductor material is narrow bandgap semiconductor powder;

[0021] The narrow bandgap semiconductor material includes one or more of ALN, BN, BP and SiP;

[0022] The conductive powder includes AZO powder doped with metal oxide;

[0023] The metal oxide includes one or more of titanium dioxide, zirconium oxide and indium oxide.

[0024] Preferably, the silane coupling agent includes one or more of A-1871, KH550, KH560, KBM303 and Z6030;

[0025] The curing agent includes a polyetheramine modified epoxy curing agent;

[0026] The accelerator includes a phenol accelerator;

[0027] The ESC dielectric layer material is specifically an ESC dielectric layer material for an aluminum substrate.

[0028] The present invention provides a method for preparing an ESC dielectric layer material as described in any one of the above technical solutions, comprising the following steps:

[0029] 1) mixing the preheated bisphenol F epoxy resin, the preheated modified epoxy resin and the preheated acrylic rubber / epoxy resin composite material, adding alumina, a narrow bandgap semiconductor material, a conductive powder and a silane coupling agent, mixing again, then adding a curing agent and continuing to mix, and finally adding an accelerator and continuing to mix to obtain a mixture;

[0030] 2) The mixture obtained in the above steps is heated and cured to obtain an ESC dielectric layer material.

[0031] Preferably, the preheating time is 1 to 2 hours;

[0032] The preheating temperature is 50-80°C;

[0033] The mixing method includes stirring and mixing with a dispersion plate;

[0034] The mixing speed is 800-1200 r / min;

[0035] The mixing time is 1 to 2 hours;

[0036] The speed of the second mixing is 800-1200 r / min;

[0037] The remixing time is 1 to 2 hours.

[0038] Preferably, the rotation speed of the continued mixing is 800-1200 r / min;

[0039] The mixing time is 0.1 to 0.2 hours;

[0040] The continuous mixing speed is 800-1200 r / min;

[0041] The continuous mixing time is 1 to 5 minutes;

[0042] The temperature of the heating curing is 80-100°C;

[0043] The heating and curing time is 1 to 3 hours.

[0044] The present invention provides the use of the ESC dielectric layer material described in any one of the above technical solutions or the ESC dielectric layer material prepared by the preparation method described in any one of the above technical solutions in an ESC substrate.

[0045] The present invention provides an ESC substrate, comprising a substrate, an intermediate layer composited on the substrate, and a dielectric layer composited on the intermediate layer;

[0046] The dielectric layer is the ESC dielectric layer material described in any one of the above technical solutions or the ESC dielectric layer material prepared by the preparation method described in any one of the above technical solutions.

[0047] Preferably, the intermediate layer includes one or more of a high temperature adhesive connection layer, a PEEK insulating film and a silver electrode;

[0048] The thickness of the dielectric layer is 200-300 μm.

[0049] The invention provides an ESC dielectric layer material, which comprises, by weight of raw materials, 10 to 25 parts by weight of bisphenol F epoxy resin, 5 to 30 parts by weight of modified epoxy resin, 5 to 15 parts by weight of acrylic rubber / epoxy resin composite material, 10 to 20 parts by weight of aluminum oxide, 5 to 25 parts by weight of narrow bandgap semiconductor material, 5 to 25 parts by weight of conductive powder, 1 to 5 parts by weight of silane coupling agent, 20 to 30 parts by weight of curing agent and 1 to 5 parts by weight of accelerator. Compared with the prior art, the present invention specially designs a material based on epoxy resin with a specific composition and ratio for the ESC dielectric layer of an aluminum substrate. Through the combination of a specific bisphenol F epoxy resin and a modified epoxy resin, the material has low surface resistance, strong adhesion and processability after curing; and combined with the selection and ratio of conductive powders, through a reasonable combination of multiple conductive powders, the material can generate JR force when power is applied, thereby achieving stable adsorption of the target object. After coating, the material only needs to be heated and cured to obtain an ESC dielectric layer with high and long-lasting adsorption force.

[0050] The components of the material provided by the present invention, which can obtain an ESC dielectric layer with high adsorption force and long-lasting adsorption force by heating and curing based on epoxy resin after coating, cooperate with each other to make the prepared adhesive have good self-defoaming ability before curing, and can obtain a relatively low surface resistivity compared to ordinary epoxy adhesives after curing, and have strong adhesion to Peek film, aluminum plate, silver and other materials, as well as machinability and grindability. It can be used for the dielectric layer of domestic aluminum substrate ESC, and can make the ESC have a high and long-lasting adsorption force. The addition of a variety of conductive powders effectively controls the resistance of the epoxy adhesive, so that the ESC as a dielectric layer can generate JR force with the adsorbed substance when power is turned on, so as to achieve adsorption of the target object. Moreover, the preparation process is simple, easy to control, and the conditions are mild, which is more conducive to the promotion and application of industrial large-scale production.

[0051] Experimental results show that the epoxy resin provided by the present invention can be used as the material of the ESC dielectric layer of the aluminum substrate, and when applied to the ESC dielectric layer, the strength and durability of the adsorption force can be significantly improved. DETAILED DESCRIPTION

[0052] In order to further understand the present invention, preferred embodiments of the present invention are described below in conjunction with examples, but it should be understood that these descriptions are only for further illustrating the features and advantages of the present invention, rather than limiting the claims of the invention.

[0053] All raw materials of the present invention have no particular limitation on their sources, and can be purchased from the market or prepared according to conventional methods known to those skilled in the art.

[0054] There is no particular restriction on the purity of all raw materials in the present invention. The present invention preferably uses analytically pure materials or materials with conventional purity requirements in the field of ESC (electrostatic chuck) dielectric layer material preparation.

[0055] The brands and abbreviations of all raw materials of the present invention are conventional brands and abbreviations in the art. Each brand and abbreviation is clear and definite in the field of its related use. Those skilled in the art can purchase them from the market or prepare them by conventional methods according to the brands, abbreviations and corresponding uses.

[0056] The present invention provides an ESC dielectric layer material, which comprises, by raw material mass fraction:

[0057] 10-25 parts by weight of bisphenol F epoxy resin;

[0058] 5 to 30 parts by weight of modified epoxy resin;

[0059] 5 to 15 parts by weight of acrylic rubber / epoxy resin composite material;

[0060] 10 to 20 parts by weight of aluminum oxide;

[0061] 5 to 25 parts by weight of narrow bandgap semiconductor material;

[0062] 5 to 25 parts by weight of conductive powder;

[0063] 1 to 5 parts by weight of silane coupling agent;

[0064] 20 to 30 parts by weight of curing agent;

[0065] Accelerator 1 to 5 parts by weight.

[0066] In the present invention, the added amount of the bisphenol F epoxy resin is 10 to 25 parts by weight, can be 13 to 23 parts by weight, can be 15 to 20 parts by weight.

[0067] In the present invention, the added amount of the modified epoxy resin is 5 to 30 parts by weight, can be 10 to 25 parts by weight, can be 15 to 20 parts by weight.

[0068] In the present invention, the added amount of the acrylic rubber / epoxy resin composite material is 5 to 15 parts by weight, can be 7 to 13 parts by weight, and can be 9 to 11 parts by weight.

[0069] In the present invention, the amount of aluminum oxide added is 10 to 20 parts by weight, can be 12 to 18 parts by weight, can be 14 to 16 parts by weight.

[0070] In the present invention, the addition amount of the narrow bandgap semiconductor material is 5 to 25 parts by weight, can be 9 to 20 parts by weight, and can be 14 to 15 parts by weight.

[0071] In the present invention, the added amount of the conductive powder is 5 to 25 parts by weight, can be 9 to 20 parts by weight, or can be 14 to 15 parts by weight.

[0072] In the present invention, the added amount of the silane coupling agent is 1 to 5 parts by weight, can be 1.5 to 4.5 parts by weight, can be 2 to 4 parts by weight, can be 2.5 to 3.5 parts by weight.

[0073] In the present invention, the added amount of the curing agent is 20 to 30 parts by weight, can be 22 to 28 parts by weight, can be 24 to 26 parts by weight.

[0074] In the present invention, the amount of the accelerator added is 1 to 5 parts by weight, can be 1.5 to 4.5 parts by weight, can be 2 to 4 parts by weight, can be 2.5 to 3.5 parts by weight.

[0075] In the present invention, the ESC dielectric layer material is preferably a material used for the ESC dielectric layer of an aluminum substrate.

[0076] In the present invention, the modified epoxy resin is preferably boron novolac epoxy resin and / or bisphenol A pentylene novolac epoxy resin, more preferably boron novolac epoxy resin or bisphenol A pentylene novolac epoxy resin.

[0077] In the present invention, the acrylic rubber / epoxy resin composite material is preferably acrylic rubber microparticles dispersed epoxy resin. Specifically, the acrylic rubber microparticles dispersed epoxy resin is ACRYSET TM .

[0078] In the present invention, the narrow bandgap semiconductor material is preferably narrow bandgap semiconductor powder.

[0079] In the present invention, the narrow bandgap semiconductor material preferably includes one or more of ALN, BN, BP and SiP, and more preferably ALN, BN, BP or SiP.

[0080] In the present invention, the conductive powder preferably includes conductive powder doped with metal oxide and semiconductor powder, and more preferably AZO (aluminum-doped zinc oxide) powder doped with metal oxide.

[0081] In the present invention, the metal oxide preferably includes one or more of titanium dioxide, zirconium oxide and indium oxide, and more preferably titanium dioxide, zirconium oxide or indium oxide.

[0082] In the present invention, the silane coupling agent preferably includes one or more of A-1871, KH550, KH560, KBM303 and Z6030, and more preferably A-1871, KH550, KH560, KBM303 or Z6030.

[0083] In the present invention, the curing agent preferably includes a polyetheramine-modified epoxy curing agent, and more preferably a phenolic-modified polyetheramine-type epoxy resin curing agent.

[0084] In the present invention, the accelerator preferably includes a phenol accelerator, and specifically, it may be 2,4,6-tris(dimethylaminomethyl)phenol.

[0085] In the present invention, the ESC dielectric layer material is preferably an ESC dielectric layer material for an aluminum substrate.

[0086] The present invention provides a method for preparing an ESC dielectric layer material as described in any one of the above technical solutions, comprising the following steps:

[0087] 1) mixing the preheated bisphenol F epoxy resin, the preheated modified epoxy resin and the preheated acrylic rubber / epoxy resin composite material, adding alumina, a narrow bandgap semiconductor material, a conductive powder and a silane coupling agent, mixing again, then adding a curing agent and continuing to mix, and finally adding an accelerator and continuing to mix to obtain a mixture;

[0088] 2) The mixture obtained in the above steps is heated and cured to obtain an ESC dielectric layer material.

[0089] The invention firstly mixes preheated bisphenol F epoxy resin, preheated modified epoxy resin and preheated acrylic rubber / epoxy resin composite material, then adds aluminum oxide, narrow bandgap semiconductor material, conductive powder and silane coupling agent and mixes them again, then adds curing agent and continues mixing, and finally adds accelerator and continues mixing to obtain a mixture.

[0090] In the present invention, the preheating time is preferably 1 to 2 hours, more preferably 1.2 to 1.8 hours, and more preferably 1.4 to 1.6 hours.

[0091] In the present invention, the preheating temperature is preferably 50-80°C, more preferably 55-75°C, more preferably 60-70°C, and specifically may be 60°C.

[0092] In the present invention, the mixing method preferably includes stirring and mixing with a dispersion disk.

[0093] In the present invention, the mixing rotation speed is preferably 800 to 1200 r / min, more preferably 850 to 1150 r / min, more preferably 900 to 1100 r / min, and more preferably 950 to 1050 r / min.

[0094] In the present invention, the mixing time is preferably 1 to 2 hours, more preferably 1.2 to 1.8 hours, and more preferably 1.4 to 1.6 hours.

[0095] In the present invention, the rotation speed of the secondary mixing is preferably 800 to 1200 r / min, more preferably 850 to 1150 r / min, more preferably 900 to 1100 r / min, and more preferably 950 to 1050 r / min.

[0096] In the present invention, the remixing time is preferably 1 to 2 hours, more preferably 1.2 to 1.8 hours, and more preferably 1.4 to 1.6 hours.

[0097] In the present invention, the rotation speed of the continued mixing is preferably 800 to 1200 r / min, more preferably 850 to 1150 r / min, more preferably 900 to 1100 r / min, and more preferably 950 to 1050 r / min.

[0098] In the present invention, the continuous mixing time is preferably 0.1 to 0.2 h, more preferably 0.12 to 0.18 h, and more preferably 0.14 to 0.16 h.

[0099] In the present invention, the rotation speed of the continuous mixing is preferably 800-1200 r / min, more preferably 850-1150 r / min, more preferably 900-1100 r / min, and more preferably 950-1050 r / min.

[0100] In the present invention, the continuous mixing time is preferably 1 to 5 min, more preferably 1.5 to 4.5 min, more preferably 2 to 4 min, and more preferably 2.5 to 3.5 min.

[0101] The present invention provides the use of the ESC dielectric layer material described in any one of the above technical solutions or the ESC dielectric layer material prepared by the preparation method described in any one of the above technical solutions in an ESC substrate.

[0102] The present invention provides an ESC (electrostatic chuck) substrate, comprising a substrate, an intermediate layer composited on the substrate, and a dielectric layer composited on the intermediate layer;

[0103] The dielectric layer is the ESC dielectric layer material described in any one of the above technical solutions or the ESC dielectric layer material prepared by the preparation method described in any one of the above technical solutions.

[0104] In the present invention, the intermediate layer preferably includes one or more of a high temperature adhesive connection layer, a PEEK insulating film and a silver electrode, and more preferably includes a high temperature adhesive connection layer, a PEEK insulating film and a silver electrode.

[0105] In the present invention, the thickness of the dielectric layer is preferably 200-300 μm, more preferably 220-280 μm, more preferably 240-260 μm. Specifically, it can be 250 μm, which is the coating thickness and the thickness after curing, and the difference between the thickness before and after curing is small.

[0106] The present invention is to complete and refine the overall technical solution, better ensure the composition and structure of the ESC dielectric layer material, and further improve the adsorption, processability and grindability of the ESC dielectric layer material. The above-mentioned epoxy resin-based material for the aluminum substrate ESC dielectric layer and its preparation method and application may specifically include the following contents:

[0107] The present invention provides an ESC dielectric layer material with high and lasting adsorption force obtained by heating and curing based on epoxy resin after coating. The material comprises the following components in parts by weight: 15-25 parts of bisphenol F epoxy resin, 5-30 parts of modified epoxy resin, 10-20 parts of acrylic rubber microparticle dispersed epoxy resin, 10-20 parts of aluminum oxide, 5-25 parts of narrow bandgap semiconductor powder, 5-25 parts of AZO powder doped with metal oxide, 1-5 parts of silane coupling agent, 20-30 parts of modified polyetheramine epoxy curing agent and 1-5 parts of phenol accelerator.

[0108] The present invention also provides a method for preparing the material of the ESC dielectric layer, comprising the following steps:

[0109] Step S1, blending of raw materials

[0110] After preheating bisphenol F epoxy resin, modified epoxy resin, and acrylic rubber microparticle dispersed epoxy resin in a 60°C oven for 1-2 hours, weigh the three raw materials in order according to their weight fractions, and then stir them for 1-2 hours using a dispersion plate at 800-1200 r / min. Then, add alumina, narrow bandgap semiconductor powder, AZO powder doped with metal oxide, and silane coupling agent in order according to their weight fractions, and then stir them for 1-2 hours using a dispersion plate at 800-1200 r / min.

[0111] The modified polyetheramine epoxy curing agent is added thereto according to its weight fraction and then stirred for 0.1-0.2h using a dispersion disk at 800-1200r / min; subsequently, the phenol accelerator is added thereto according to its weight fraction and then stirred for 1-5min using a dispersion disk at 800-1200r / min.

[0112] Specifically, the modified epoxy resin is at least one of boron novolac epoxy resin and BPA-GA (bisphenol A pentanediol novolac epoxy resin).

[0113] Specifically, the narrow bandgap semiconductor material is at least one of ALN, BN, BP, and SiP.

[0114] Specifically, the metal oxide-doped AZO powder is a type of conductive powder obtained by mixing (at least one of titanium dioxide, zirconium oxide and indium oxide) with soluble aluminum salt and zinc oxide salt using a sol-gel method and undergoing drying, sintering and grinding.

[0115] Specifically, in step S2, after all components are fully mixed, vacuum is evacuated to remove bubbles, so as to obtain the epoxy adhesive product of the ESC dielectric layer with high and long-lasting adsorption force, which can be obtained by heating and curing after coating.

[0116] Specifically, in step S3, the finished adhesive is coated on the ESC substrate with a coating thickness of 250 μm, and after coating, it is placed in an oven for heating and curing.

[0117] Specifically, the curing temperature is 80 to 100° C., and the curing time is 1 to 3 hours.

[0118] The above content of the present invention provides a material based on epoxy resin for aluminum substrate ESC dielectric layer and its preparation method and application. The present invention specially designs the material based on epoxy resin for aluminum substrate ESC dielectric layer with specific composition and ratio. Through the combination of specific bisphenol F epoxy resin and modified epoxy resin, the material has low surface resistance, strong adhesion and processability after curing; and combined with the selection and ratio of conductive powder, through the reasonable combination of multiple conductive powders, the material can generate JR force when powered on, and realize stable adsorption of the target object. After coating, the material only needs to be heated and cured to obtain an ESC dielectric layer with high adsorption force and long-lasting adsorption force.

[0119] The components of the material provided by the present invention, which can obtain an ESC dielectric layer with high adsorption force and long-lasting adsorption force by heating and curing based on epoxy resin after coating, cooperate with each other to make the prepared adhesive have good self-defoaming ability before curing, and can obtain a relatively low surface resistivity compared to ordinary epoxy adhesives after curing, and have strong adhesion to Peek film, aluminum plate, silver and other materials, as well as machinability and grindability. It can be used for the dielectric layer of domestic aluminum substrate ESC, and can make the ESC have a high and long-lasting adsorption force. The addition of a variety of conductive powders effectively controls the resistance of the epoxy adhesive, so that the ESC as a dielectric layer can generate JR force with the adsorbed substance when power is turned on, so as to achieve adsorption of the target object. Moreover, the preparation process is simple, easy to control, and the conditions are mild, which is more conducive to the promotion and application of industrial large-scale production.

[0120] Experimental results show that the epoxy resin provided by the present invention can be used as the material of the ESC dielectric layer of the aluminum substrate, and when applied to the ESC dielectric layer, the strength and durability of the adsorption force can be significantly improved.

[0121] In order to further illustrate the present invention, an ESC dielectric layer material and a preparation method, application, and an ESC substrate provided by the present invention are described in detail in combination with embodiments below. However, it should be understood that these embodiments are implemented on the premise of the technical solution of the present invention, and detailed implementation methods and specific operating processes are given only to further illustrate the features and advantages of the present invention, rather than to limit the claims of the present invention. The protection scope of the present invention is not limited to the following embodiments.

[0122] Example 1

[0123] This embodiment provides a material for an ESC dielectric layer with high and long-lasting adsorption force, which is based on epoxy resin and can be obtained by heating and curing after coating. The material comprises the following components in parts by weight:

[0124] 20 parts of bisphenol F epoxy resin, 15 parts of boron phenolic epoxy resin, 5 parts of acrylic rubber microparticle dispersed epoxy resin, 10 parts of alumina, 15 parts of ALN powder, 10 parts of AZO conductive powder doped with zirconium oxide, 3 parts of KH560 coupling agent, 20 parts of phenolic modified polyether amine epoxy curing agent, and 2 parts of 2,4,6-tris(dimethylaminomethyl)phenol.

[0125] Preparation process:

[0126] 1. Preheat bisphenol F epoxy resin, boron phenolic epoxy resin, and acrylic rubber microparticle dispersed epoxy resin in a 60°C oven for 1 hour, weigh the three raw materials in order according to their weight fractions, and then stir them at 800 r / min on a dispersion plate for 2 hours. Then add alumina, ALN powder, AZO conductive powder doped with zirconium oxide, and KH560 in order according to their weight fractions, and then stir them at 800 r / min on a dispersion plate for 2 hours. Add phenolic modified polyether amine epoxy curing agent in accordance with its weight fraction, and then stir it at 800 r / min on a dispersion plate for 0.2 hours; then add 2,4,6-tris(dimethylaminomethyl)phenol in accordance with its weight fraction and stir it at 800 r / min on a dispersion plate for 5 minutes;

[0127] 2. After all components are fully mixed, vacuum is evacuated to remove bubbles and obtain the finished material.

[0128] Example 2

[0129] This embodiment provides an epoxy adhesive that can be used as an ESC dielectric layer of an aluminum substrate after being heated and cured, comprising the following components in parts by weight:

[0130] 13 parts of bisphenol F epoxy resin, 15 parts of bisphenol A pentanediol epoxy resin, 12 parts of acrylic rubber microparticle dispersed epoxy resin, 10 parts of alumina, 5 parts of ALN, 5 parts of BP, 15 parts of AZO conductive powder doped with indium oxide, 2 parts of A-1871 coupling agent, 20 parts of phenolic modified polyether amine epoxy curing agent, and 3 parts of 2,4,6-tris(dimethylaminomethyl)phenol.

[0131] Preparation process:

[0132] 1. Preheat bisphenol F epoxy resin, bisphenol A pentanediol epoxy resin, and acrylic rubber microparticle dispersed epoxy resin in a 60°C oven for 1.25 hours, weigh the three raw materials in order according to their weight fractions, and then stir them at 900 r / min on a dispersion plate for 1.5 hours. Then, add alumina, ALN, BP, indium oxide-doped AZO conductive powder, and A-1871 in order according to their weight fractions, and then stir them at 900 r / min on a dispersion plate for 1.75 hours. Add phenolic modified polyether amine epoxy curing agent in accordance with its weight fraction, and then stir it at 900 r / min on a dispersion plate for 0.175 hours; then add 2,4,6-tris(dimethylaminomethyl)phenol in accordance with its weight fraction and stir it at 900 r / min on a dispersion plate for 4 minutes;

[0133] 2. After all components are fully mixed, vacuum is evacuated to remove bubbles and obtain the finished material.

[0134] Example 3

[0135] This embodiment provides a material for an ESC dielectric layer with high and long-lasting adsorption force, which is based on epoxy resin and can be obtained by heating and curing after coating. The material comprises the following components in parts by weight:

[0136] 22 parts of bisphenol F epoxy resin, 20 parts of boron phenolic epoxy resin, 5 parts of acrylic rubber microparticle dispersed epoxy resin, 10 parts of alumina, 5 parts of BN, 10 parts of AZO conductive powder doped with titanium dioxide, 2 parts of KBM303 coupling agent, 23 parts of phenolic modified polyether amine epoxy curing agent, and 2 parts of 2,4,6-tris(dimethylaminomethyl)phenol.

[0137] Preparation process:

[0138] 1. Preheat bisphenol F epoxy resin, boron phenolic epoxy resin, and acrylic rubber microparticle dispersed epoxy resin in a 60°C oven for 1.5 hours, weigh the three raw materials in order according to their weight fractions, and then use a dispersion plate to stir at 1000 r / min for 1.5 hours. Then add alumina, BN powder, titanium dioxide-doped AZO conductive powder, and KBM303 in order according to their weight fractions, and then use a dispersion plate to stir at 1000 r / min for 1.5 hours. Add phenolic modified polyether amine epoxy curing agent according to its weight fraction, and then use a dispersion plate to stir at 1000 r / min; then add 2,4,6-tris(dimethylaminomethyl)phenol according to its weight fraction and use a dispersion plate to stir at 1000 r / min for 3 minutes;

[0139] 2. After all components are fully mixed, vacuum is evacuated to remove bubbles and obtain the finished material.

[0140] Comparative Example 1

[0141] This comparative example provides a material for an ESC dielectric layer based on epoxy resin, comprising the following components in parts by weight:

[0142] 35 parts of bisphenol F epoxy resin, 15 parts of acrylic rubber microparticle dispersed epoxy resin, 10 parts of alumina, 15 parts of ALN, 10 parts of AZO conductive powder doped with zirconium oxide, 3 parts of KH550 coupling agent, 25 parts of phenolic modified polyether amine epoxy curing agent, and 2 parts of 2,4,6-tris(dimethylaminomethyl)phenol.

[0143] Preparation process:

[0144] 1. Preheat bisphenol F epoxy resin, boron phenolic epoxy resin, and acrylic rubber microparticle dispersed epoxy resin in a 60°C oven for 1 hour, weigh the three raw materials in order according to their weight fractions, and then stir them at 800 r / min on a dispersion plate for 2 hours. Then add alumina, ALN powder, AZO conductive powder doped with zirconium oxide, and KH550 in order according to their weight fractions, and then stir them at 800 r / min on a dispersion plate for 2 hours. Add phenolic modified polyether amine epoxy curing agent in accordance with its weight fraction and stir it at 800 r / min on a dispersion plate for 0.2 hours; then add 2,4,6-tris(dimethylaminomethyl)phenol in accordance with its weight fraction and stir it at 800 r / min on a dispersion plate for 5 minutes;

[0145] 2. After all components are fully mixed, vacuum is evacuated to remove bubbles and obtain the finished material.

[0146] Comparative Example 2

[0147] This comparative example provides a material for an ESC dielectric layer, comprising the following components in parts by weight:

[0148] 20 parts of bisphenol F epoxy resin, 15 parts of boron novolac epoxy resin, 5 parts of acrylic rubber microparticle dispersed epoxy resin, 25 parts of aluminum oxide, 10 parts of AZO conductive powder doped with indium oxide, 3 parts of Z6030 coupling agent, 20 parts of phenolic modified polyether amine epoxy curing agent, and 2 parts of 2,4,6-tris(dimethylaminomethyl)phenol.

[0149] Preparation process:

[0150] 1. Preheat bisphenol F epoxy resin, boron phenolic epoxy resin, and acrylic rubber microparticle dispersed epoxy resin in a 60°C oven for 1 hour, weigh the three raw materials in order according to their weight fractions, and then stir them at 800 r / min on a dispersion plate for 2 hours. Then add alumina, indium oxide-doped AZO conductive powder, and Z6030 in order according to their weight fractions, and then stir them at 800 r / min on a dispersion plate for 2 hours. Add phenolic modified polyether amine epoxy curing agent in accordance with its weight fraction and stir it at 800 r / min on a dispersion plate for 0.2 hours; then add 2,4,6-tris(dimethylaminomethyl)phenol in accordance with its weight fraction and stir it at 800 r / min on a dispersion plate for 5 minutes;

[0151] 2. After all components are fully mixed, vacuum is evacuated to remove bubbles and obtain the finished material.

[0152] Comparative Example 3

[0153] This comparative example provides a material for an ESC dielectric layer, comprising the following components in parts by weight:

[0154] 20 parts of bisphenol F epoxy resin, 15 parts of bisphenol A pentanediol epoxy resin, 5 parts of acrylic rubber microparticle dispersed epoxy resin, 20 parts of alumina, 5 parts of SiP, 10 parts of ALN, 3 parts of KH560 coupling agent, 20 parts of phenolic modified polyether amine epoxy curing agent, and 2 parts of 2,4,6-tris(dimethylaminomethyl)phenol.

[0155] Preparation process:

[0156] 1. Preheat bisphenol F epoxy resin, bisphenol A pentanediol epoxy resin, and acrylic rubber microparticle dispersed epoxy resin in a 60°C oven for 1 hour, weigh the three raw materials in order according to their weight fractions, and then stir them at 800 r / min on a dispersion plate for 2 hours. Then add alumina, SiP, ALN, and KH560 in order according to their weight fractions, and then stir them at 800 r / min on a dispersion plate for 2 hours. Add phenolic modified polyether amine epoxy curing agent in accordance with its weight fraction and stir it at 800 r / min on a dispersion plate for 0.2 hours; then add 2,4,6-tris(dimethylaminomethyl)phenol in accordance with its weight fraction and stir it at 800 r / min on a dispersion plate for 5 minutes;

[0157] 2. After all components are fully mixed, vacuum is evacuated to remove bubbles and obtain the finished material.

[0158] In order to further illustrate that the dielectric layer prepared by heating and curing in various embodiments of the present invention can improve the strength and durability of the ESC adsorption force, relevant performance tests were conducted on Examples 1 to 3 and Comparative Examples 1 to 3, and the test methods are as follows:

[0159] The finished adhesive in each example was passed through a polytetrafluoroethylene mold, heated at 80° C. for 2 hours, and made into a disc with a diameter of 10 cm and a thickness of 1 mm to test its surface resistance.

[0160] Each example is coated on the ESC substrate with a thickness of 250μm, then cured in an 80-degree oven for 2 hours. After curing, it is left overnight. The next day, the adsorption force of the ESC substrate on the polarizer is tested at 1KV. The substrate is placed in a constant temperature and humidity chamber at 20℃ and 55% humidity, and the adsorption force is tested every two months.

[0161] The test results are shown in Table 1, which shows the performance data of the ESC substrates prepared in the examples and comparative examples of the present invention.

[0162] Table 1

[0163]

[0164] As can be seen from Table 1, the epoxy resin-based material disclosed in the embodiment of the present invention can be used as the ESC dielectric layer of the aluminum substrate. When applied to the ESC dielectric layer, the strength and durability of its adsorption force can be significantly improved.

[0165] It can also be seen from Table 1 that when no modified epoxy resin is added to Comparative Example 1, although a lower resistance value and a higher adsorption force can be obtained initially, the adsorption force decays over time.

[0166] In comparative example 2, no narrow bandgap semiconductor material is added, and the resistance value of the dielectric layer increases significantly, resulting in a significant decrease in the adsorption force.

[0167] In comparative example 3, no conductive powder is added, which also significantly increases the resistance value of the dielectric layer, thereby causing a significant decrease in the adsorption force.

[0168] The above is a detailed introduction to a material for an ESC dielectric layer of an aluminum substrate based on epoxy resin provided by the present invention and a preparation method thereof. The principle and implementation method of the present invention are described in this article using specific examples. The description of the above embodiments is only used to help understand the method of the present invention and its core ideas, including the best mode, and also enables any technician in the field to practice the present invention, including the manufacture and use of any device or system, and the implementation of any combined method. It should be pointed out that for ordinary technicians in this technical field, without departing from the principle of the present invention, several improvements and modifications can be made to the present invention, and these improvements and modifications also fall within the scope of protection of the claims of the present invention. The scope of patent protection of the present invention is defined by the claims and may include other embodiments that can be thought of by those skilled in the art. If these other embodiments have structural elements that are not different from the literal expression of the claims, or if they include equivalent structural elements that are not substantially different from the literal expression of the claims, then these other embodiments should also be included in the scope of the claims.

Claims

1. An ESC dielectric layer material, characterized in that: Calculated by raw material mass fraction, including: 10-25 parts by weight of bisphenol F epoxy resin; 5 to 30 parts by weight of modified epoxy resin; 5 to 15 parts by weight of acrylic rubber / epoxy resin composite material; 10-20 parts by weight of aluminum oxide; 5 to 25 parts by weight of narrow bandgap semiconductor material; 5 to 25 parts by weight of conductive powder; 1 to 5 parts by weight of silane coupling agent; 20 to 30 parts by weight of curing agent; Accelerator 1 to 5 parts by weight.

2. The ESC dielectric layer material according to claim 1, characterized in that: The ESC dielectric layer material is a material used for the ESC dielectric layer of an aluminum substrate; The modified epoxy resin is boron novolac epoxy resin and / or bisphenol A pentyl novolac epoxy resin; The acrylic rubber / epoxy resin composite material is acrylic rubber particles dispersed in epoxy resin.

3. The ESC dielectric layer material according to claim 1, characterized in that: The narrow bandgap semiconductor material is narrow bandgap semiconductor powder; The narrow bandgap semiconductor material includes one or more of ALN, BN, BP and SiP; The conductive powder includes AZO powder doped with metal oxide; The metal oxide includes one or more of titanium dioxide, zirconium oxide and indium oxide.

4. The ESC dielectric layer material according to claim 1, characterized in that: The silane coupling agent includes one or more of A-1871, KH550, KH560, KBM303 and Z6030; The curing agent includes a polyetheramine modified epoxy curing agent; The accelerator includes a phenol accelerator; The ESC dielectric layer material is specifically an ESC dielectric layer material for an aluminum substrate.

5. A method for preparing an ESC dielectric layer material according to any one of claims 1 to 4, characterized in that: The following steps are involved: 1) mixing the preheated bisphenol F epoxy resin, the preheated modified epoxy resin and the preheated acrylic rubber / epoxy resin composite material, adding alumina, a narrow bandgap semiconductor material, a conductive powder and a silane coupling agent, mixing again, then adding a curing agent and continuing to mix, and finally adding an accelerator and continuing to mix to obtain a mixture; 2) The mixture obtained in the above steps is heated and cured to obtain an ESC dielectric layer material.

6. The preparation method according to claim 5, characterized in that: The preheating time is 1 to 2 hours; The preheating temperature is 50-80°C; The mixing method includes stirring and mixing with a dispersion plate; The mixing speed is 800-1200 r / min; The mixing time is 1 to 2 hours; The speed of the second mixing is 800-1200 r / min; The remixing time is 1 to 2 hours.

7. The preparation method according to claim 5, characterized in that: The rotating speed of the continuous mixing is 800-1200 r / min; The mixing time is 0.1 to 0.2 hours; The continuous mixing speed is 800-1200 r / min; The continuous mixing time is 1 to 5 minutes; The temperature of the heating curing is 80-100°C; The heating and curing time is 1 to 3 hours.

8. Use of the ESC dielectric layer material according to any one of claims 1 to 4 or the ESC dielectric layer material prepared by the preparation method according to any one of claims 5 to 7 in an ESC substrate.

9. An ESC substrate, characterized in that: It includes a substrate, an intermediate layer compounded on the substrate, and a dielectric layer compounded on the intermediate layer; The dielectric layer is the ESC dielectric layer material according to any one of claims 1 to 4 or the ESC dielectric layer material prepared by the preparation method according to any one of claims 5 to 8.

10. The ESC substrate according to claim 9, characterized in that: The intermediate layer includes one or more of a high temperature adhesive connection layer, a PEEK insulating film and a silver electrode; The thickness of the dielectric layer is 200-300 μm.

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