CN103013042A - Metamaterial dielectric substrate and processing method thereof - Google Patents
Metamaterial dielectric substrate and processing method thereof Download PDFInfo
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- CN103013042A CN103013042A CN2011102969196A CN201110296919A CN103013042A CN 103013042 A CN103013042 A CN 103013042A CN 2011102969196 A CN2011102969196 A CN 2011102969196A CN 201110296919 A CN201110296919 A CN 201110296919A CN 103013042 A CN103013042 A CN 103013042A
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- mesoporous silicon
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Abstract
The invention provides a metamaterial dielectric substrate and a processing method thereof. The processing method comprises the following steps of: (101) preparing mesoporous silicon dioxide; (102) preparing a mesoporous silicon dioxide and epoxy resin composite material; and (103) forming the metamaterial dielectric substrate through carrying out hot-pressing on the mesoporous silicon dioxide and epoxy resin composite material. According to the metamaterial dielectric substrate and the processing method of the metamaterial dielectric substrate, the composite material is prepared from an organic macromolecular material and a porous material, and the metamaterial dielectric substrate is then synthesized, so that the dielectric constant of the metamaterial dielectric substrate can be greatly reduced, the mechanical property of the dielectric substrate is enhanced, and the prepared metamaterial dielectric substrate is better in comprehensive performance and meets the requirements of the modern packaging material substrate, thereby having good development and application prospects.
Description
[technical field]
The present invention relates to super Material Field, relate to particularly a kind of super material medium substrate and working method thereof.
[background technology]
Super material is generally folded by a plurality of super material function flaggies or is formed by other rule array combination, super material function plate comprises medium substrate and the array a plurality of artificial microstructure on medium substrate, the medium substrate of existing super material is the organic or inorganic substrate of uniform material, such as FR4, TP1 etc.The a plurality of artificial microstructure of array on medium substrate has specific electromagnetic property, can produce electromagnetic response to electric field or magnetic field, accurately design and control by structure and arrangement regulation to artificial microstructure, can make super material present the electromagnetic property that various general material does not have, if converge, disperse and deviation hertzian wave etc.
Resins, epoxy is the organic high molecular compound that contains two or more epoxide groups in the general reference molecule, Resins, epoxy has very strong force of cohesion, molecular structure is fine and close, so its mechanical property is higher, dielectric properties are good, and its product size good stability, hardness is high, snappiness is better, to alkali and most of solvent-stable, is widely used in social production, the life.Commercial high frequency substrate mainly contains three major types at present: tetrafluoroethylene (PTFE) substrate, thermosetting polyphenylene ether (Polyphenyl Oxide), interlinkage polyhutadiene substrate and Resins, epoxy composite base plate (FR-4).Wherein the specific inductivity of ptfe substrate is 2.1-10.6, and the specific inductivity of Resins, epoxy composite base plate is 4.2-5.4.
Mesoporous material is because its special pore passage structure and higher specific surface area and thermostability, have a wide range of applications in fields such as catalysis, separation, the research of mesoporous material has become the study hotspot of numerous ambits such as striding in the world physics, chemistry, material, biology and information and has studied one of forward position.In recent years, educational circles gives great concern to the research of mesoporous material, is that mesoporous material has carried out more deep research to silicon especially.Find that according to existing achievement in research the mesoporous silica film that silicon-dioxide is made has special dimensional effect, can be at sensor, low dielectric constant interlayer, once the aspects such as permeable membrane, multilayer film and optical material had huge application prospect.
The modern electronic technology fast development, the processing of digital circuit, transmission enter the high frequency stage, the quality of substrate performance will produce material impact to circuit characteristic this moment, wherein several the indexs such as dielectric properties, thermotolerance, dimensional stability, wet fastness are particularly important, and the performance quality of substrate depends primarily on employed baseplate material, and therefore selecting high performance baseplate material is the prerequisite of preparation high-performance substrate.
The resin of tradition preparation substrate adopts resol and Resins, epoxy more, at present most popular is the Resins, epoxy FR-4 that glass fibre strengthens, this material is because manufacturing cost is lower so that cost performance is higher, in the low-frequency electronic product, have preferably and use, but in high frequency circuit,, resistance to elevated temperatures lower because of its dielectric properties is relatively poor not to be suitable in the high frequency circuit, prepare the high-quality substrate that meets super material package processing requirement that specific inductivity is lower, mechanical property is superior, can adopt the method preparation of synthetic composite material.
[summary of the invention]
Technical problem to be solved by this invention provides a kind of medium substrate and working method thereof of super material, and the medium substrate of processing by this method has lower specific inductivity, and mechanical property has good exploitation and application prospect preferably.
The present invention realizes that goal of the invention at first provides a kind of medium substrate and working method thereof of super material, may further comprise the steps:
101. preparation mesoporous silicon oxide;
102. preparation mesoporous silicon oxide-epoxy resin composite material;
103. mesoporous silicon oxide-epoxy resin composite material is hot pressed into super material medium substrate.
In the preparation of step 101 intermediary hole SiO 2 powder, adopt following methods:
1011. hydrochloric acid soln and polyoxyethylene-poly-oxypropylene polyoxyethylene triblock copolymer are placed four-hole boiling flask, and heated and stirred is even;
1012. the tetraethoxy heated and stirred is even, slowly inject above-mentioned mixing solutions;
1013. will put into the hydrothermal reaction kettle crystallization behind the solution left standstill, sedimentation and filtration, washing, the drying of crystallization is placed in the muffle furnace and calcines, obtain mesoporous silicon oxide.
As preferred embodiment, in the described step 1011, the concentration of described hydrochloric acid soln is controlled at 1-5mol/L.
As preferred embodiment, in the described step 1012, the temperature of described tetraethoxy heating is controlled at 30-60 ℃.
As preferred embodiment, in the described step 1013, described crystallization temperature is controlled at 90-120 ℃, and crystallization time is controlled at 20-30h.
As preferred embodiment, in the described step 1013, described calcining temperature is controlled at 450-650 ℃, and calcination time is controlled at 5-10h.
In step 102, preparation mesoporous silicon oxide-epoxy resin composite material may further comprise the steps:
1021. with the mesoporous silicon oxide hydrophobically modified, mesoporous silicon oxide is placed beaker, add silane coupling agent, disperse post-heating to stir with ultrasonic wave, obtain the mesoporous silicon oxide after the modification after centrifugal, the washing;
1022. with the heating of Resins, epoxy, epoxy resin diluent, add while stirring mesoporous silicon oxide, methyl hexahydrobenzene acyl after the modification, desolventizing obtains mesoporous silicon oxide-epoxy resin composite material.
As preferred embodiment, in the described step 1021, described silane coupling agent is γ-aminopropyl triethoxysilane or γ-methacryloxypropyl trimethoxy silane, and the mass ratio that adds silane coupling agent is 0.1%-1.2%wt.
As preferred embodiment, in the described step 1022, the mass ratio of mesoporous silicon oxide and Resins, epoxy is 60-80: 40-20 after the described adding modification.
As preferred embodiment, in the described step 1022, the add-on of described methyl hexahydrophthalic anhydride is the 1%-45wt% of Resins, epoxy add-on.
As preferred embodiment, in the described step 1022, described epoxy resin diluent is acetone, benzene,toluene,xylene.
As preferred embodiment, in the described step 103, the temperature of described hot pressing is 50-370 ℃, and the pressure of hot pressing is 5-50MPa.
A kind of super material medium substrate is composited by the mesoporous silicon oxide after the modification and Resins, epoxy, and the mesoporous silicon oxide after the modification and the mass ratio of Resins, epoxy are 60-80: 40-20.
Use working method of the present invention mesoporous silicon oxide and Resins, epoxy are made matrix material, be hot pressed into medium substrate, the specific inductivity of Resins, epoxy is lower, good heat resistance, after adding mesoporous silicon oxide, greatly strengthened the mechanical property of matrix material, the medium substrate of processing by this method has lower specific inductivity, mechanical property has good exploitation and application prospect preferably.
[description of drawings]
Fig. 1, super material medium base plate processing method schema.
Fig. 2, mesoporous silicon oxide preparation flow figure.
Fig. 3, mesoporous silicon oxide-epoxy resin composite material preparation flow figure.
[embodiment]
The present invention is described in detail below in conjunction with drawings and Examples.
The present invention is compounded to form organic/inorganic composite porous advanced low-k materials with organic polymer material Resins, epoxy and porous material mesoporous silicon oxide, again matrix material is made super material medium substrate, the medium substrate that makes combines the characteristics of above-mentioned bi-material, has lower specific inductivity and superior mechanical property.Simultaneously, this complete processing is simple and easy to do, and is lower for the requirement of processing environment and experimental installation, is easy to realize.
Embodiment 1
The working method of present embodiment is as follows:
The preparation mesoporous silicon oxide:
1011. be that 2mol/L hydrochloric acid soln and 4g polyoxyethylene-poly-oxypropylene polyoxyethylene triblock copolymer place four-hole boiling flask with 160ml concentration, be heated to 40 ℃, stir 1.5h, form colourless transparent solution;
1012. the 8.5g tetraethoxy is heated to 40 ℃, stir 1.5h, slowly inject above-mentioned mixing solutions;
1013. will put into the hydrothermal reaction kettle crystallization behind the solution left standstill 24h, crystallization temperature is controlled at 110 ℃ of sedimentation and filtrations with crystallization, washing, drying and is placed in the muffle furnace and calcines, temperature in the muffle furnace is controlled at 500 ℃, and calcination time is controlled at 6h, can obtain mesoporous silicon oxide.
Preparation mesoporous silicon oxide-epoxy resin composite material:
1021. with the mesoporous silicon oxide hydrophobically modified, the 2g mesoporous silicon oxide is placed beaker, the γ-aminopropyl triethoxysilane (KH-550) that adds 0.01g, above-mentioned mixing solutions is heated to 40 ℃, disperse 10min with ultrasonic wave, be placed on and stir 2h on the magnetic stirring apparatus, mixing solutions is centrifugal as clean-out system with ethanol, washing obtains the mesoporous silicon oxide after the modification after 4 times;
1022. get 100ml acetone, the 1g bisphenol A type epoxy resin places beaker, beaker is placed on the agitator, be heated to 60 ℃, add while stirring mesoporous silicon oxide, 0.4g methyl hexahydrophthalic anhydride after the modification, above-mentioned mixing solutions is placed on the agitator, 80 ℃ of lower 10h that stir after the solvent evaporation in the solution to be mixed, obtain mesoporous silicon oxide and epoxy resin composite material mixture;
103. mixture is placed mould, and hot pressing forms super material medium substrate, hot pressing temperature is 180 ℃, and hot pressing pressure is 30MPa.
Should be appreciated that in the present embodiment that the temperature and pressure of hot pressing is to determine according to the kind of selected Resins, epoxy.
Embodiment 2
The preparation mesoporous silicon oxide:
1011. be that 2mol/L hydrochloric acid soln and 4g polyoxyethylene-poly-oxypropylene polyoxyethylene triblock copolymer place four-hole boiling flask with 160ml concentration, be heated to 40 ℃, stir 1.5h, form colourless transparent solution;
1012. the 8.5g tetraethoxy is heated to 40 ℃, stir 1.5h, slowly inject above-mentioned mixing solutions;
1013. will put into the hydrothermal reaction kettle crystallization behind the solution left standstill 24h, crystallization temperature is controlled at 110 ℃ of sedimentation and filtrations with crystallization, washing, drying and is placed in the muffle furnace and calcines, temperature in the muffle furnace is controlled at 500 ℃, and calcination time is controlled at 6h, can obtain mesoporous silicon oxide.
Preparation mesoporous silicon oxide-epoxy resin composite material:
1021. with the mesoporous silicon oxide hydrophobically modified, the 3g mesoporous silicon oxide is placed beaker, γ-the methacryloxypropyl trimethoxy silane (KH-570) that adds 0.03g, above-mentioned mixing solutions is heated to 40 ℃, disperse 10min with ultrasonic wave, be placed on and stir 2h on the magnetic stirring apparatus, mixing solutions is centrifugal as clean-out system with ethanol, washing obtains the mesoporous silicon oxide after the modification after 3 times;
1022. get 200ml acetone, the 1.5g bisphenol A type epoxy resin places beaker, beaker is placed on the agitator, be heated to 80 ℃, add while stirring mesoporous silicon oxide, 0.6g methyl hexahydrophthalic anhydride after the modification, above-mentioned mixing solutions is placed on the agitator, 80 ℃ of lower 16h that stir after the solvent evaporation in the solution to be mixed, obtain mesoporous silicon oxide and epoxy resin composite material mixture;
103. mixture is placed mould, and hot pressing forms super material medium substrate, hot pressing temperature is 180 ℃, and hot pressing pressure is 45MPa.
Above-described embodiment among the present invention has only been done exemplary description, and those skilled in the art can carry out various modifications to the present invention in the situation that does not break away from the spirit and scope of the present invention after reading present patent application.
Claims (13)
1. the working method of a super material medium substrate is characterized in that, may further comprise the steps,
101. preparation mesoporous silicon oxide;
102. preparation mesoporous silicon oxide-epoxy resin composite material;
103. mesoporous silicon oxide-epoxy resin composite material is hot pressed into super material medium substrate.
2. the working method of super material medium substrate according to claim 1 is characterized in that, in the described step 101, described preparation mesoporous silicon oxide may further comprise the steps,
1011. hydrochloric acid soln and polyoxyethylene-poly-oxypropylene polyoxyethylene triblock copolymer are placed four-hole boiling flask, and heated and stirred is even;
1012. the tetraethoxy heated and stirred is even, slowly inject above-mentioned mixing solutions;
1013. will put into the hydrothermal reaction kettle crystallization behind the solution left standstill, sedimentation and filtration, washing, the drying of crystallization is placed in the muffle furnace and calcines, obtain mesoporous silicon oxide.
3. the working method of super material medium substrate according to claim 2 is characterized in that, in the described step 1011, the concentration of described hydrochloric acid soln is controlled at 1-5mol/L.
4. the working method of super material medium substrate according to claim 2 is characterized in that, in the described step 1012, the temperature of described tetraethoxy heating is controlled at 30-60 ℃.
5. the working method of super material medium substrate according to claim 2 is characterized in that, in the described step 1013, described crystallization temperature is controlled at 90-120 ℃, and crystallization time is controlled at 20-30h.
6. the working method of super material medium substrate according to claim 2 is characterized in that, in the described step 1013, described calcining temperature is controlled at 450-650 ℃, and calcination time is controlled at 5-10h.
7. the working method of super material medium substrate according to claim 1 is characterized in that, in the described step 102, described preparation mesoporous silicon oxide-epoxy resin composite material may further comprise the steps,
1021. with the mesoporous silicon oxide hydrophobically modified, mesoporous silicon oxide is placed beaker, add silane coupling agent, disperse post-heating to stir with ultrasonic wave, obtain the mesoporous silicon oxide after the modification after centrifugal, the washing;
1022. with the heating of Resins, epoxy, epoxy resin diluent, add while stirring mesoporous silicon oxide, methyl hexahydrobenzene acyl after the modification, desolventizing obtains mesoporous silicon oxide-epoxy resin composite material.
8. the working method of super material medium substrate according to claim 7, it is characterized in that, in the described step 1021, described silane coupling agent is γ-aminopropyl triethoxysilane or γ-methacryloxypropyl trimethoxy silane, and the mass ratio that adds silane coupling agent is 0.1%-1.2%.
9. the working method of super material medium substrate according to claim 7 is characterized in that, in the described step 1022, the mass ratio of mesoporous silicon oxide and Resins, epoxy is 60-80: 40-20 after the described adding modification.
10. the working method of super material medium substrate according to claim 7 is characterized in that, in the described step 1022, the add-on of described methyl hexahydrophthalic anhydride is the 1%-45wt% of Resins, epoxy add-on.
11. the working method of super material medium substrate according to claim 7 is characterized in that, in the described step 1022, described epoxy resin diluent is acetone, benzene,toluene,xylene.
12. the working method of super material medium substrate according to claim 1 is characterized in that, in the described step 103, the temperature of described hot pressing is 50-370 ℃, and the pressure of hot pressing is 5-50MPa.
13. a super material medium substrate is characterized in that, mesoporous silicon oxide and the Resins, epoxy of described medium substrate after by modification is composited, and the mesoporous silicon oxide after the described modification and the mass ratio of Resins, epoxy are 60-80: 40-20.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104004386A (en) * | 2014-06-06 | 2014-08-27 | 宁波高新区夏远科技有限公司 | Preparation method of modified nano SiO2 and polyvinyl chloride (PVC) composition |
| CN107603157A (en) * | 2017-10-20 | 2018-01-19 | 福建师范大学 | A kind of Janus bulking agents for rubber-toughened epoxy resin and preparation method thereof |
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| US7965219B1 (en) * | 2009-09-24 | 2011-06-21 | The Boeing Company | Patterned optical material and metamaterial for protection from and defeat of directed energy |
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| CN1783357A (en) * | 2004-11-30 | 2006-06-07 | 财团法人工业技术研究院 | Modified mesoporous silicon dioxide powder, presolution for forming low dielectric opoxy resin and low dielectric polysub amido resin, low dielectric constant base board and its forming method |
| US7965219B1 (en) * | 2009-09-24 | 2011-06-21 | The Boeing Company | Patterned optical material and metamaterial for protection from and defeat of directed energy |
Non-Patent Citations (1)
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104004386A (en) * | 2014-06-06 | 2014-08-27 | 宁波高新区夏远科技有限公司 | Preparation method of modified nano SiO2 and polyvinyl chloride (PVC) composition |
| CN104004386B (en) * | 2014-06-06 | 2015-07-29 | 宁波高新区夏远科技有限公司 | The preparation method of modified Nano SiO2 and polychloroethylene composition |
| CN107603157A (en) * | 2017-10-20 | 2018-01-19 | 福建师范大学 | A kind of Janus bulking agents for rubber-toughened epoxy resin and preparation method thereof |
| CN107603157B (en) * | 2017-10-20 | 2019-04-30 | 福建师范大学 | A kind of Janus expanding material and preparation method thereof for rubber-toughened epoxy resin |
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