CN104693684A - Adhesive, organic ceramic plate and preparation method of organic ceramic plate - Google Patents
Adhesive, organic ceramic plate and preparation method of organic ceramic plate Download PDFInfo
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- CN104693684A CN104693684A CN201510100997.2A CN201510100997A CN104693684A CN 104693684 A CN104693684 A CN 104693684A CN 201510100997 A CN201510100997 A CN 201510100997A CN 104693684 A CN104693684 A CN 104693684A
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Abstract
The invention provides an adhesive, an organic ceramic plate and a preparation method of the organic ceramic plate. The adhesive comprises the following components in percentage by mass: 10-30% of epoxy resin, 10-30% of thermosetting phenol formaldehyde resin, 3-5% of latent curing agent, 0.5-1% of epoxy resin curing accelerator, 10-30% of inorganic filler, 10-20% of toughener, 0.5-2% of thixotropic agent, 0.5-2% of silane coupling agent and 35-45% of diluting solvent. When the adhesive is used in an organic ceramic plate preparation process, the adhesive and ceramic powder can be precured into a solid at low temperature (generally 50-80 DEG C), and pulverized into granules, thereby ensuring the smooth proceeding of the hot pressing of the organic ceramic plate. In the curing process of the plate subjected to hot pressing, the latent curing agent and epoxy resin curing accelerator can quickly cure the epoxy resin in a short time, thereby ensuring the formation of the organic ceramic plate and enhancing the performance of the formed organic ceramic plate.
Description
Technical field
The present invention relates to shaped material field, in particular to the preparation method of a kind of tackiness agent, organic ceramic plate and organic ceramic plate.
Background technology
Organic ceramic plate is that one utilizes thermal conductive ceramic powder and organic binder bond as raw material, and prepare under low temperature (being generally less than 200 DEG C) condition meet the organic composite ceramic substrate that heat conducting circuit board requires.It has high heat conduction, high-insulativity, can meet the performances such as great power LED cooling requirement, its substrate as the copper-clad plate of organic ceramic base is used, and is widely used in the fields such as electronics, communication, illumination, equipment.
Tackiness agent is that one uses, for helping shaping auxiliary agent in material or product (such as organic ceramic plate) moulding process.Tackiness agent is often made up of various ingredients, but basic function composition mainly contains three parts, i.e. major ingredient, auxiliary agent and solvent.Major ingredient as tackiness agent has a variety of, is generally superpolymer, as polyvinyl alcohol, polyvinyl formal etc.Auxiliary agent is generally the reagent that can play toughness reinforcing plasticization effect after adding to tackiness agent and use system thereof, as the series such as aromatic ester, polyglycol.Solvent role dissolves all major ingredients and auxiliary agent, and major ingredient and auxiliary agent determine kind and the consumption of used solvent.The solvent of tackiness agent can for common are machine solvent, such as toluene, acetone, ethanol, butanols or hexanaphthene etc.
At present, existing tackiness agent (as epoxy resin, resol, polyvinyl alcohol etc.) can not meet the production technique of organic ceramic base copper-clad plate, namely can not be solid by mixed slurry Procuring when removing the solvent be mixed to get by ceramic powder and tackiness agent in mixed slurry, and then cannot pulverize as particle, and then cannot hot pressing be the sheet material of even material, and obtained organic ceramic plate intensity is poor, heat conductivility, resistance to elevated temperatures do not reach normal usage level.Meanwhile, the second-order transition temperature (Tg) of existing adhesive composition is low, and in printed circuit board processing and use procedure, ability of anti-deformation is poor.For the problems referred to above, also there is no effective solution at present.
Summary of the invention
The present invention aims to provide the preparation method of a kind of tackiness agent, organic ceramic plate and organic ceramic plate, to improve the performance of the organic ceramic plate utilizing tackiness agent to be formed.
To achieve these goals, according to an aspect of the present invention, provide a kind of tackiness agent, by percentage to the quality, tackiness agent comprises following component: the epoxy resin of 10 ~ 30%, the heat-reactive phenolic resin of 10 ~ 30%, 3 ~ 5% latent curing agent, 0.5% ~ 1% epoxy resin curing accelerator, 10 ~ 30% mineral filler, the toughner of 10 ~ 20%, thixotropic agent, the silane coupling agent of 0.5 ~ 2%, the diluting solvent of 35 ~ 45% of 0.5 ~ 2%.
Further, epoxy resin by any one in E44 type epoxy resin, E51 type epoxy resin, and 4, any one compound composition in 4 '-diaminodiphenylmethane epoxy resin and p-aminophenol epoxy resin.
Further, latent curing agent is selected from any one or more in 4,4-diaminodiphenylsulfone(DDS), Dyhard RU 100, hydrazides and methyl tetrahydro phthalic anhydride.
Further, epoxy resin curing accelerator is selected from glyoxal ethyline and/or substituted urea.
Further, mineral filler is inorganic oxide.
Further, mineral filler is selected from any one or more in aluminum oxide, silicon oxide and titanium oxide.
Further, toughner is paracril.
Further, thixotropic agent is thermal silica and/or vapor phase process aluminum oxide.
Further, diluting solvent is ethyl acetate or acetone.
Meanwhile, present invention also offers a kind of preparation method of organic ceramic plate, this preparation method comprises the following steps: mixed to obtain mixed slurry with tackiness agent provided by the invention by ceramic powder; Procuring is carried out with the diluting solvent removed in tackiness agent to mixed slurry and obtains solid-state material; Solid-state material is ground into mixed powder, and mixed powder is carried out hot-forming to obtain sheet material; Sheet material is carried out backflow solidification to obtain organic ceramic plate.
Further, the temperature of Procuring is 50 ~ 80 DEG C.
Further, the temperature of backflow solidification is 120 ~ 150 DEG C, and the time of backflow solidification is 5 ~ 15min.
Further, ceramic powder is Al
2o
3or AlN.
Meanwhile, present invention also offers a kind of organic ceramic plate, be mixed to form by tackiness agent and stupalith, this tackiness agent is tackiness agent provided by the invention.
Apply technical scheme of the present invention, the invention provides a kind of tackiness agent comprising epoxy resin, heat-reactive phenolic resin, latent curing agent, epoxy resin curing accelerator, mineral filler, toughner, thixotropic agent, silane coupling agent and diluting solvent.Latent curing agent in this tackiness agent and epoxy resin curing accelerator can ensure that tackiness agent preserves the long period at normal temperatures; Be used for by this tackiness agent in the preparation process of organic ceramic plate, tackiness agent and ceramic powder can Procuring be solid under low temperature (being generally 50-80 DEG C), then pulverize as particle, thus ensure that the hot-forming of organic ceramic plate is carried out smoothly; Be cured in process to the sheet material of hot-forming rear acquisition, latent curing agent and epoxy resin curing accelerator be rapid solidification epoxy resin at short notice, ensure that the shaping of organic ceramic plate, and improve the performance of formed organic ceramic plate.
Embodiment
It should be noted that, when not conflicting, the embodiment in the application and the feature in embodiment can combine mutually.The present invention is described in detail below in conjunction with embodiment.
It should be noted that used term is only to describe embodiment here, and be not intended to the illustrative embodiments of restricted root according to the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative is also intended to comprise plural form, in addition, it is to be further understood that, " comprise " when using term in this manual and/or " comprising " time, it indicates existing characteristics, step, operation, device, assembly and/or their combination.
Technology of having powerful connections is known, existing tackiness agent can not meet the production technique of organic ceramic base copper-clad plate, namely can not be solid by mixed slurry Procuring when removing the solvent be mixed to get by ceramic powder and tackiness agent in mixed slurry, and then cannot pulverize as particle, and then cannot hot pressing be the sheet material of even material, and obtained organic ceramic plate intensity is poor, heat conductivility, resistance to elevated temperatures does not reach normal usage level effect poor in ceramic powder low temperature moulding, obtained organic ceramic plate intensity is poor, and its heat conductivility, resistance to sparking can not reach normal usage level.The present inventor studies for the problems referred to above, provides a kind of tackiness agent.By percentage to the quality, tackiness agent comprises following component: the epoxy resin of 10 ~ 30%, the heat-reactive phenolic resin of 10 ~ 30%, 3 ~ 5% latent curing agent, 0.5% ~ 1% epoxy resin curing accelerator, 10 ~ 30% mineral filler, the toughner of 10 ~ 20%, thixotropic agent, the silane coupling agent of 0.5 ~ 2%, the diluting solvent of 35 ~ 45% of 0.5 ~ 2%.
Latent curing agent in above-mentioned tackiness agent and epoxy resin curing accelerator can ensure that tackiness agent preserves the long period at normal temperatures; Be used for by this tackiness agent in the preparation process of organic ceramic plate, tackiness agent and ceramic powder can Procuring be solid under low temperature (being generally 50-80 DEG C), then pulverize as particle, thus ensure that the hot-forming of organic ceramic plate is carried out smoothly; Be cured in process to the sheet material of hot-forming rear acquisition, latent curing agent and epoxy resin curing accelerator be rapid solidification epoxy resin at short notice, ensure that the shaping of organic ceramic plate, and improve the performance of formed organic ceramic plate.
Illustrative embodiments according to tackiness agent provided by the invention will be described in more detail below.But these illustrative embodiments can be implemented by multiple different form, and should not be interpreted as being only limited to embodiment set forth herein.Should be understood that, provide these embodiments be in order to make the application open thorough and complete, and the design of these illustrative embodiments is fully conveyed to those of ordinary skill in the art.
In above-mentioned tackiness agent, the kind of epoxy resin can set according to the actual requirements.Preferably, further, epoxy resin is by any one in E44 type epoxy resin, E51 type epoxy resin, and 4, any one compound composition in 4 '-diaminodiphenylmethane epoxy resin and p-aminophenol epoxy resin, this is because E series epoxy resins glass transition temperature Tg is low, Tg is high for AG-80, AG-90 epoxy resin, compound use.Certainly, the kind of epoxy resin is not limited to above-described embodiment.
Heat-reactive phenolic resin can at 50 ~ 80 DEG C Procuring epoxy resin, and there is no the generation of moisture, whole system can be made to become solid and pulverize, obtain hot pressing particle; Can with the crosslinked structure of epoxy resin height of formation in cured later process, this individual system had both maintained the good adhesivity of epoxy resin, maintained again the thermotolerance of resol, make resol/epoxy resin can at 260 DEG C life-time service.This tackiness agent epoxy resin palpus thermosetting modification resol is composite, plays Procuring effect.
Latent curing agent not cured epoxy resin at normal temperatures, only just cured epoxy resin under the conditions of cure such as certain heat, light, makes this tackiness agent be able to long-term room-temperature preservation.Preferably, latent curing agent is selected from any one or more in 4,4-diaminodiphenylsulfone(DDS), Dyhard RU 100, hydrazides and methyl tetrahydro phthalic anhydride.
Epoxy resin curing accelerator uses for coordinating latent curing agent, and (such as at a certain temperature) can make rapid solidification in the epoxy-resin systems short period of time under specific condition of cure.Preferably, epoxy resin curing accelerator is selected from glyoxal ethyline and/or substituted urea.
In order to improve heat conductivility and the mechanical property of the organic ceramic plate utilizing this tackiness agent to be formed, above-mentioned tackiness agent also comprises mineral filler.Mineral filler can be inorganic oxide, and preferably, mineral filler is selected from any one or more in aluminum oxide, silicon oxide and titanium oxide.Certainly, mineral filler can also be other fillers, such as aluminium nitride etc.
In order to give tackiness agent good thixotropy, above-mentioned tackiness agent also comprises thixotropic agent.The kind of thixotropic agent can set according to the actual requirements, and preferably, thixotropic agent is thermal silica and/or vapor phase process aluminum oxide.Above-mentioned tackiness agent also comprises toughner, and toughner can adopt paracril etc.Further, tackiness agent also comprises silane coupling agent, and silane coupling agent can improve the modified effect of filler, toughner.The model that silane coupling agent can adopt this area common, such as KH-560 etc.
In addition, tackiness agent also comprises diluting solvent, for diluted system, tackiness agent is mixed better with ceramic powder.The kind of diluting solvent has a lot, and preferably, diluting solvent is ethyl acetate or acetone.It should be noted that contriver just obtains the content (and massfraction) of each component in above-mentioned tackiness agent by lot of experiments after having paid creative work.In actual process process, after weighing each component according to component concentration provided by the invention, fully mix to obtain with agitator and state tackiness agent.Meanwhile, contriver finds after experimental study, and the performance of the organic ceramic plate utilizing the tackiness agent of above-mentioned content to be formed is significantly improved.
Present invention also offers a kind of preparation method of organic ceramic plate, this preparation method comprises the following steps: mixed to obtain mixed slurry with tackiness agent provided by the invention by ceramic powder; Procuring is carried out with the diluting solvent removed in tackiness agent to mixed slurry and obtains solid-state material; Solid-state material is ground into mixed powder, and mixed powder is carried out hot-forming to obtain sheet material; Sheet material is carried out backflow solidification to obtain organic ceramic plate.
In above-mentioned preparation method, tackiness agent and ceramic powder can Procuring be solid under low temperature (being generally 50-80 DEG C), then pulverize as particle, thus ensure that the hot-forming of organic ceramic plate is carried out smoothly; Be cured in process to the sheet material of hot-forming rear acquisition, latent curing agent and epoxy resin curing accelerator be rapid solidification epoxy resin at short notice, ensure that the shaping of organic ceramic plate, and improve the performance of formed organic ceramic plate.
The illustrative embodiments of preparation method will described in more detail according to organic ceramic plate provided by the invention below.But these illustrative embodiments can be implemented by multiple different form, and should not be interpreted as being only limited to embodiment set forth herein.Should be understood that, provide these embodiments be in order to make the application open thorough and complete, and the design of these illustrative embodiments is fully conveyed to those of ordinary skill in the art.
First, ceramic powder is mixed to obtain mixed slurry with tackiness agent provided by the invention.In this step, need ceramic powder fully to mix with tackiness agent provided by the invention.Wherein, ceramic powder can adopt material common in this area, and preferably, ceramic powder is Al
2o
3or AlN.
Then, Procuring is carried out with the diluting solvent removed in tackiness agent to mixed slurry and obtain solid-state material.The temperature of Procuring is relevant to the kind of diluting solvent.Preferably the temperature of Procuring is 50 ~ 80 DEG C.
Next, solid-state material is ground into mixed powder, and mixed powder is carried out hot-forming to obtain sheet material.Hot-forming referring to applies pressure to mixed powder at a certain temperature, thus makes mixed powder shaping.Hot-forming actual process parameter with reference to prior art, can not repeat them here.
Finally, sheet material is carried out backflow solidification to obtain organic ceramic plate.The processing condition of backflow solidification can set according to actual process demand, and preferably, backflow solidification value is 120 ~ 150 DEG C, and backflow set time is 5 ~ 15min.Namely canescence organic ceramic plate is obtained after overcuring (now adhesive portion solidification).Then, organic ceramic plate carries out covering copper, temperature 150-200 DEG C, 30-60min, and now tackiness agent solidifies completely.
Meanwhile, present invention also offers a kind of organic ceramic plate, be mixed to form by tackiness agent and stupalith, this tackiness agent is tackiness agent provided by the invention.Because this organic ceramic plate is mixed to form by tackiness agent provided by the invention and stupalith, and tackiness agent and ceramic powder can Procuring be solid under low temperature (being generally 50-80 DEG C), then pulverize as particle, thus ensure that the hot-forming of organic ceramic plate is carried out smoothly; Be cured in process to the sheet material of hot-forming rear acquisition, latent curing agent and epoxy resin curing accelerator be rapid solidification epoxy resin at short notice, ensure that the shaping of organic ceramic plate, and improve the performance of formed organic ceramic plate.
The preparation method of tackiness agent provided by the invention and organic ceramic plate is further illustrated below in conjunction with embodiment.
Embodiment 1
By percentage to the quality, the tackiness agent that the present embodiment provides comprises following component: the E44 type epoxy resin of 10%, 20% 4,4 '-diaminodiphenylmethane epoxy resin, the heat-reactive phenolic resin of 10%, 4,4-diaminodiphenylsulfone(DDS)s, the substituted urea of 1%, aluminum oxide, the paracril of 10%, thermal silica, the silane coupling agent (KH-560) of 0.5%, the ethyl acetate of 33% of 0.5% of 10% of 5%.
The preparation method of the organic ceramic plate that the present embodiment provides comprises the following steps: by Al
2o
3powder mixes to obtain mixed slurry with above-mentioned tackiness agent; Carry out Procuring with the diluting solvent removed in tackiness agent to mixed slurry and obtain solid-state material, wherein, the temperature of Procuring is 60 DEG C; Solid-state material is ground into mixed powder, and mixed powder is carried out hot-forming to obtain sheet material; Obtain organic ceramic plate after being solidified by sheet material, solidification value is 150 DEG C, and set time is 10min.
The thermal conductivity of the organic ceramic plate that test the present embodiment obtains, its thermal conductivity is 3.5W/mK.After the organic ceramic plate obtained by the present embodiment is placed in 260 DEG C of solder bath 2min, organic ceramic plate is non-foaming, not stratified.Meanwhile, the flexural strength also obtaining organic ceramic plate after tested can reach 40N/mm, and the Tg of organic ceramic plate can reach 180 DEG C.
Embodiment 2
By percentage to the quality, the tackiness agent that the present embodiment provides comprises following component: the E51 type epoxy resin of 5%, the p-aminophenol epoxy resin of 5%, the heat-reactive phenolic resin of 26.5%, Dyhard RU 100, the substituted urea of 0.5%, aluminum oxide, the paracril of 12%, thermal silica, the silane coupling agent (KH-560) of 1%, the ethyl acetate of 35% of 1% of 11% of 3%.
The preparation method of the organic ceramic plate that the present embodiment provides comprises the following steps: mixed to obtain mixed slurry with above-mentioned tackiness agent by AlN powder; Carry out Procuring with the diluting solvent removed in tackiness agent to mixed slurry and obtain solid-state material, wherein, the temperature of Procuring is 80 DEG C; Solid-state material is ground into mixed powder, and mixed powder is carried out hot-forming to obtain sheet material; Obtain organic ceramic plate after being solidified by sheet material, solidification value is 120 DEG C, and set time is 15min.
The thermal conductivity of the organic ceramic plate that test the present embodiment obtains, its thermal conductivity is 3.8W/mK.After the organic ceramic plate obtained by the present embodiment is placed in 260 DEG C of solder bath 2min, organic ceramic plate is non-foaming, not stratified.Meanwhile, the flexural strength also obtaining organic ceramic plate after tested can reach 42N/mm, and the Tg of organic ceramic plate can reach 200 DEG C.
Embodiment 3
By percentage to the quality, the tackiness agent that the present embodiment provides comprises following component: the E44 type epoxy resin of 5%, 5% 4,4 '-diaminodiphenylmethane epoxy resin, the heat-reactive phenolic resin of 10%, hydrazides, the glyoxal ethyline of 1%, silicon oxide, the paracril of 10%, thermal silica, the silane coupling agent (KH-560) of 2%, the ethyl acetate of 45% of 2% of 16% of 4%.
The preparation method of the organic ceramic plate that the present embodiment provides comprises the following steps: by Al
2o
3powder mixes to obtain mixed slurry with above-mentioned tackiness agent; Carry out Procuring with the diluting solvent removed in tackiness agent to mixed slurry and obtain solid-state material, wherein, the temperature of Procuring is 70 DEG C; Mixed powder is carried out hot-forming to obtain sheet material; Obtain organic ceramic plate after being solidified by sheet material, solidification value is 100 DEG C, and set time is 4min.
The thermal conductivity of the organic ceramic plate that test the present embodiment obtains, its thermal conductivity is 4.5W/mK.After the organic ceramic plate obtained by the present embodiment is placed in 260 DEG C of solder bath 2min, organic ceramic plate is non-foaming, not stratified.Meanwhile, the flexural strength also obtaining organic ceramic plate after tested can reach 50N/mm, and the Tg of organic ceramic plate can reach 200 DEG C.
Embodiment 4
By percentage to the quality, the tackiness agent that the present embodiment provides comprises following component: the E51 type epoxy resin of 5%, the p-aminophenol epoxy resin of 5%, the heat-reactive phenolic resin of 30%, methyl tetrahydro phthalic anhydride, the glyoxal ethyline of 1%, silicon oxide, the paracril of 10%, thermal silica, the silane coupling agent (KH-560) of 0.5%, the ethyl acetate of 35% of 0.5% of 10% of 3%.
The preparation method of the organic ceramic plate that the present embodiment provides comprises the following steps: by Al
2o
3powder mixes to obtain mixed slurry with above-mentioned tackiness agent; Carry out Procuring with the diluting solvent removed in tackiness agent to mixed slurry and obtain solid-state material, wherein, the temperature of Procuring is 80 DEG C; Mixed powder is carried out hot-forming to obtain sheet material; Obtain organic ceramic plate after being solidified by sheet material, solidification value is 150 DEG C, and set time is 5min.
The thermal conductivity of the organic ceramic plate that test the present embodiment obtains, its thermal conductivity is 4.2W/mK.After the organic ceramic plate obtained by the present embodiment is placed in 260 DEG C of solder bath 2min, organic ceramic plate is non-foaming, not stratified.Meanwhile, the flexural strength also obtaining organic ceramic plate after tested can reach 30N/mm, and the Tg of organic ceramic plate can reach 200 DEG C.
Embodiment 5
By percentage to the quality, the tackiness agent that the present embodiment provides comprises following component: the E44 type epoxy resin of 5%, the p-aminophenol epoxy resin of 5%, the heat-reactive phenolic resin of 10%, Dyhard RU 100, the glyoxal ethyline of 1%, titanium oxide, the paracril of 10%, thermal silica, the silane coupling agent (KH-560) of 0.5%, the ethyl acetate of 35% of 0.5% of 30% of 3%.
The preparation method of the organic ceramic plate that the present embodiment provides comprises the following steps: by Al
2o
3powder mixes to obtain mixed slurry with above-mentioned tackiness agent; Carry out Procuring with the diluting solvent removed in tackiness agent to mixed slurry and obtain solid-state material, wherein, the temperature of Procuring is 70 DEG C; Mixed powder is carried out hot-forming to obtain sheet material; Obtain organic ceramic plate after being solidified by sheet material, solidification value is 100 DEG C, and set time is 10min.
The thermal conductivity of the organic ceramic plate that test the present embodiment obtains, its thermal conductivity is 4.7W/mK.After the organic ceramic plate obtained by the present embodiment is placed in 260 DEG C of solder bath 2min, organic ceramic plate is non-foaming, not stratified.Meanwhile, the flexural strength also obtaining organic ceramic plate after tested can reach 45N/mm, and the Tg of organic ceramic plate can reach 200 DEG C.
Embodiment 6
By percentage to the quality, the tackiness agent that the present embodiment provides comprises following component: the E44 type epoxy resin of 5%, 5% 4,4 '-diaminodiphenylmethane epoxy resin, the heat-reactive phenolic resin of 10%, Dyhard RU 100, the glyoxal ethyline of 1%, titanium oxide, the paracril of 20%, gaseous oxidation aluminium, the silane coupling agent (KH-560) of 0.5%, the acetone of 35% of 0.5% of 10% of 3%.
The preparation method of the organic ceramic plate that the present embodiment provides comprises the following steps: by Al
2o
3powder mixes to obtain mixed slurry with above-mentioned tackiness agent; Carry out Procuring with the diluting solvent removed in tackiness agent to mixed slurry and obtain solid-state material, wherein, the temperature of Procuring is 70 DEG C; Mixed powder is carried out hot-forming to obtain sheet material; Obtain organic ceramic plate after being solidified by sheet material, solidification value is 100 DEG C, and set time is 10min.
The thermal conductivity of the organic ceramic plate that test the present embodiment obtains, its thermal conductivity is 5W/mK.Meanwhile, after the organic ceramic plate obtained by the present embodiment is placed in 260 DEG C of solder bath 2min, organic ceramic plate is non-foaming, not stratified.Meanwhile, the flexural strength also obtaining organic ceramic plate after tested can reach 35N/mm, and the Tg of organic ceramic plate can reach 200 DEG C.
Comparative example 1
By percentage to the quality, the tackiness agent that this comparative example provides comprises following component: the bisphenol A epoxide resin of 34%, the thixotropic agent of 1%, 65% diluting solvent.
The preparation method of the organic ceramic plate that the present embodiment provides comprises the following steps: by Al
2o
3powder mixes to obtain mixed slurry with above-mentioned tackiness agent; Carry out Procuring with the diluting solvent removed in tackiness agent to mixed slurry and obtain solid-state material, wherein, the temperature of Procuring is 70 DEG C; Mixed powder is carried out hot-forming to obtain sheet material; Obtain organic ceramic plate after being solidified by sheet material, solidification value is 100 DEG C, and set time is 10min.
Test the thermal conductivity of the organic ceramic plate that this comparative example obtains, its thermal conductivity is 2.1W/mK.After the organic ceramic plate obtained by the present embodiment is placed in 260 DEG C of solder bath 2min, organic ceramic plate generating portion is bubbled, layering.Meanwhile, the flexural strength also obtaining organic ceramic plate after tested can reach 21N/mm, and the Tg of organic ceramic plate can reach 154 DEG C.
As can be seen from the above embodiments, the thermal conductivity of the organic ceramic plate that embodiment 1 to 6 obtains is 3.5 ~ 5W/mK, and the thermal conductivity of the organic ceramic plate that comparative example 1 obtains is 2.1W/mK, the thermal conductivity of the organic ceramic plate that the thermal conductivity of the organic ceramic plate that visible embodiment 1 to 6 obtains obtains apparently higher than comparative example 1.In addition, the organic ceramic plate that embodiment 1 to 6 obtains is all non-foaming, not stratified after thermal shock test, and comparative example 1 organic ceramic plate generating portion after thermal shock test is bubbled, layering, the thermal shock resistance properties of the organic ceramic plate that the thermal shock resistance properties executing the organic ceramic plate that example 1 to 6 obtains as seen obtains apparently higher than comparative example 1.Further, the Tg of the organic ceramic plate that embodiment 1 to 6 obtains is 180-200 DEG C, and its flexural strength is 30-50/mm, far above the organic ceramic plate that comparative example obtains.
As can be seen from the above description, the above embodiments of the present invention achieve following technique effect:
(2) the invention provides a kind of tackiness agent comprising epoxy resin, heat-reactive phenolic resin, latent curing agent, epoxy resin curing accelerator, mineral filler, toughner, thixotropic agent, silane coupling agent and diluting solvent.Latent curing agent in this tackiness agent and epoxy resin curing accelerator can ensure that tackiness agent preserves the long period at normal temperatures; Be used for by this tackiness agent in the preparation process of organic ceramic plate, tackiness agent and ceramic powder can Procuring be solid under low temperature (being generally 50-80 DEG C), then pulverize as particle, thus ensure that the hot-forming of organic ceramic plate is carried out smoothly; Be cured in process to the sheet material of hot-forming rear acquisition, latent curing agent and epoxy resin curing accelerator be rapid solidification epoxy resin at short notice, ensure that the shaping of organic ceramic plate, and improve the performance of formed organic ceramic plate.
(2) this tackiness agent obtains organic ceramic base copper-clad plate Tg and can reach 150-240 DEG C, and at high temperature non-deformability is strong; This tackiness agent obtains organic ceramic base copper-clad plate flexural strength can reach 30-50/mm; This tackiness agent obtains organic ceramic base copper-clad plate thermal conductivity can reach 2-5W/mK; This this tackiness agent obtain the copper-clad plate of organic ceramic base can at 260 DEG C life-time service.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (14)
1. a tackiness agent, it is characterized in that, by percentage to the quality, described tackiness agent comprises following component: the epoxy resin of 10 ~ 30%, the heat-reactive phenolic resin of 10 ~ 30%, 3 ~ 5% latent curing agent, 0.5% ~ 1% epoxy resin curing accelerator, 10 ~ 30% mineral filler, the toughner of 10 ~ 20%, thixotropic agent, the silane coupling agent of 0.5 ~ 2%, the diluting solvent of 35 ~ 45% of 0.5 ~ 2%.
2. tackiness agent according to claim 1, it is characterized in that, described epoxy resin by any one in E44 type epoxy resin, E51 type epoxy resin, and 4, any one compound composition in 4 '-diaminodiphenylmethane epoxy resin and p-aminophenol epoxy resin.
3. tackiness agent according to claim 1 and 2, is characterized in that, described latent curing agent is selected from any one or more in 4,4-diaminodiphenylsulfone(DDS), Dyhard RU 100, hydrazides and methyl tetrahydro phthalic anhydride.
4. tackiness agent according to claim 1 and 2, is characterized in that, described epoxy resin curing accelerator is selected from glyoxal ethyline and/or substituted urea.
5. tackiness agent according to claim 1, is characterized in that, described mineral filler is inorganic oxide.
6. tackiness agent according to claim 5, is characterized in that, described mineral filler is selected from any one or more in aluminum oxide, silicon oxide and titanium oxide.
7. tackiness agent according to claim 1, is characterized in that, described toughner is paracril.
8. tackiness agent according to claim 1, is characterized in that, described thixotropic agent is thermal silica and/or vapor phase process aluminum oxide.
9. tackiness agent according to claim 1, is characterized in that, described diluting solvent is ethyl acetate or acetone.
10. a preparation method for organic ceramic plate, is characterized in that, described preparation method comprises the following steps:
Ceramic powder is mixed to obtain mixed slurry with the tackiness agent according to any one of claim 1 to 9;
Procuring is carried out with the diluting solvent removed in described tackiness agent to described mixed slurry and obtains solid-state material;
Described solid-state material is ground into mixed powder, and described mixed powder is carried out hot-forming to obtain sheet material;
Described sheet material is carried out backflow solidification to obtain described organic ceramic plate.
11. preparation methods according to claim 10, is characterized in that, the temperature of described Procuring is 50 ~ 80 DEG C.
12. preparation methods according to claim 10, is characterized in that, the temperature of described backflow solidification is 120 ~ 150 DEG C, and the time of described backflow solidification is 5 ~ 15min.
13., according to claim 10 to the preparation method according to any one of 12, is characterized in that, described ceramic powder is Al
2o
3or AlN.
14. 1 kinds of organic ceramic plates, are mixed to form by tackiness agent and stupalith, it is characterized in that, the tackiness agent of described tackiness agent according to any one of claim 1 to 9.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105753460A (en) * | 2016-02-03 | 2016-07-13 | 蒙娜丽莎集团股份有限公司 | Low-shrinkage high-strength large-scale ceramic plate and preparation method thereof |
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| CN106082781A (en) * | 2016-06-02 | 2016-11-09 | 廊坊市高瓷新材料科技有限公司 | Ceramic composition, ceramic substrate and phone housing |
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| CN107163503B (en) * | 2017-06-02 | 2020-04-07 | 江苏华海诚科新材料股份有限公司 | Epoxy resin composition suitable for packaging photoelectric coupler |
| CN109534834A (en) * | 2018-08-08 | 2019-03-29 | 中国科学院化学研究所 | One kind can ceramic phenolic resin and its preparation method and application |
| CN112142461A (en) * | 2019-06-28 | 2020-12-29 | 比亚迪股份有限公司 | Ceramic composition, ceramic, and preparation method and application thereof |
| CN113473781A (en) * | 2021-07-27 | 2021-10-01 | Oppo广东移动通信有限公司 | Shell assembly, preparation method thereof and electronic equipment |
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| CN115159994A (en) * | 2022-05-25 | 2022-10-11 | 惠州市杜科新材料有限公司 | Ceramic powder adhesive for electronic ceramics and preparation method thereof |
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