CN103059511A - Epoxy-based composite dielectric material and preparation method thereof - Google Patents
Epoxy-based composite dielectric material and preparation method thereof Download PDFInfo
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- CN103059511A CN103059511A CN2012105918843A CN201210591884A CN103059511A CN 103059511 A CN103059511 A CN 103059511A CN 2012105918843 A CN2012105918843 A CN 2012105918843A CN 201210591884 A CN201210591884 A CN 201210591884A CN 103059511 A CN103059511 A CN 103059511A
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Abstract
The invention discloses an epoxy-based composite dielectric material which comprises the following components by weight: 100 parts of epoxy resin, 40-120 parts of anhydride curing agent, 1-10 parts of curing accelerator, 10-30 parts of polyether polyol grafted modifier and 100-400 parts of filler particles. The invention further discloses a preparation method of the epoxy-based composite dielectric material. The preparation method comprises the following steps: dissolving the anhydride curing agent containing the polyether polyol grafted modifier and the curing accelerator in an organic solvent; adding the epoxy resin; adding the filler particles and obtaining a dielectric slurry; molding the dielectric slurry; and evaporating and curing the solvent by heating. According to the epoxy-based composite dielectric material and the preparation method, the polyether polyol grafted modifier is added to increase the content of a polar group of an epoxy matrix and improve the matrix polarizability, thereby improving dielectric properties of the epoxy-based composite dielectric material.
Description
Technical field
The present invention relates to the composite dielectric material field, relate in particular to a kind of epoxy group(ing) composite dielectric material and preparation method thereof.
Background technology
Along with the fast development of electronics and information industry, electronic product has towards the development trend of microminiaturization and Highgrade integration, and therefore the design for electronic devices and components has also proposed Secretary.Dielectric substance with high-k is the key of electronic devices and components microminiaturization, and it is mainly for the manufacture of high-performance buried capacitors, random access memory etc.Current this field mainly be inorganic ceramic material take high-k as main, but because the shortcoming such as the stupalith snappiness is poor, power consumption is large, manufacturing process is complicated has to a certain degree limited the application of inorganic ceramic dielectric material.Organic film dielectric substance, particularly thin-film material have good snappiness and processibility, and good imbedibility and cementability are arranged between the substrate, therefore obtain gradually paying attention to.Ceramic micro-nano granules and organic polymer matrix are carried out compound, ceramic particle and interpolymer interaction can be prepared the polymer-based carbon flexibility function matrix material with high-k.
In recent years, about the research of ceramic micro-nano granules and organic polymer matrix composite constantly is in the news, yet prior art concentrates on the method that obtains high dielectric constant by improving filler content mostly, ignored the modification to organic matrixs such as epoxies, therefore be difficult to so that the specific inductivity of matrix material further improves.
Summary of the invention
The present invention is intended to solve above-mentioned problems of the prior art, proposes a kind of epoxy group(ing) composite dielectric material and preparation method thereof.
One aspect of the present invention proposes a kind of epoxy group(ing) composite dielectric material, comprises (by weight component): 100 parts of Resins, epoxy, anhydride curing agent 40-120 part, curing catalyst 1-10 part, polyether glycol graft modification agent 10-30 part and filler particles 100-400 part.
The present invention proposes a kind of epoxy group(ing) composite dielectric material preparation method on the other hand, comprises the steps: that the anhydride curing agent that will contain polyether glycol graft modification agent and curing catalyst is dissolved in the organic solvent; Add Resins, epoxy; Add filler particles, obtain the dielectric medium slurry; Make the moulding of described dielectric medium slurry; Heating makes described solvent evaporation and solidifies.
Epoxy group(ing) composite dielectric material that the present invention proposes and preparation method thereof is by adding polyether glycol graft modification agent, increased the polar group content of epoxy matrix, improve the matrix polarizability, thereby improved the dielectric properties of described epoxy group(ing) composite dielectric material.
Description of drawings
Fig. 1 is the epoxy group(ing) composite dielectric material of one of embodiment of the invention and preparation method thereof experimental result picture;
Fig. 2 is the epoxy group(ing) composite dielectric material with one of embodiment of the invention and preparation method thereof contrast and experiment figure;
Fig. 3 is two epoxy group(ing) composite dielectric material of the embodiment of the invention and preparation method thereof experimental result picture;
Fig. 4 is three epoxy group(ing) composite dielectric material of the embodiment of the invention and preparation method thereof experimental result picture;
Fig. 5 is four epoxy group(ing) composite dielectric material of the embodiment of the invention and preparation method thereof experimental result picture.
Fig. 6 is for adding polyoxyethylene glycol and adopting the Different Weight component proportion to prepare the specific inductivity curve of electric capacity under different frequency that the epoxy group(ing) composite dielectric material is made;
Fig. 7 is for adding polyoxyethylene glycol and adopting the Different Weight component proportion to prepare the dielectric loss curve of electric capacity under different frequency that the epoxy group(ing) composite dielectric material is made;
Fig. 8 is not for to add polyoxyethylene glycol and to adopt the Different Weight component proportion to prepare the specific inductivity curve of electric capacity under different frequency that the epoxy group(ing) composite dielectric material is made;
Fig. 9 is not for to add polyoxyethylene glycol and to adopt the Different Weight component proportion to prepare the dielectric loss curve of electric capacity under different frequency that the epoxy group(ing) composite dielectric material is made;
Figure 10 adds under the 1KHZ and does not add polyoxyethylene glycol and adopt Different Weight component proportion scheme at different B aTiO
3The dielectric constant values correlation curve figure of the epoxy group(ing) composite dielectric material under the weight;
Figure 11 is the specific inductivity curve of the hybrid epoxidized composite sample of F51/221 of one embodiment of the invention;
Figure 12 is the dielectric loss curve of the hybrid epoxidized composite sample of F51/221 of one embodiment of the invention;
Figure 13 is the specific inductivity curve of the hybrid epoxidized composite sample of E51/CCTO of one embodiment of the invention;
Figure 14 is the dielectric loss curve of the hybrid epoxidized composite sample of E51/CCTO of one embodiment of the invention.
Embodiment
In order to make purpose of the present invention, technical scheme and advantage more clear, below in conjunction with drawings and Examples, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, is not intended to limit the present invention.
One aspect of the present invention has proposed a kind of epoxy group(ing) composite dielectric material, comprises (by weight component): 100 parts of Resins, epoxy, anhydride curing agent 40-120 part, curing catalyst 1-10 part, polyether glycol graft modification agent 10-30 part and filler particles 100-400 part.
Wherein, described Resins, epoxy is selected from a kind of in bisphenol A type epoxy resin, bisphenol f type epoxy resin, novolac epoxy, the cycloaliphatic epoxy resin or their arbitrary combination.
Described anhydride curing agent is selected from a kind of in Tetra hydro Phthalic anhydride, Tetra Hydro Phthalic Anhydride or its substitutive derivative (for example methyl tetrahydrophthalic anhydride), hexahydrophthalic anhydride or its substitutive derivative (for example methylhexahydrophthalic anhydride), the Pyroglutaric acid or their arbitrary combination.
Described curing catalyst is selected from a kind of in methyl ethyl diketone salt (for example acetylacetone cobalt, chromium acetylacetonate, acetylacetone copper) or the acetoacetic ester (such as methyl aceto acetate, butyl-acetoacetate).
Described polyether glycol graft modification agent is the oligopolymer of polyhydroxy-alcohol.Described polyether glycol graft modification agent includes but not limited to a kind of in polyoxyethylene glycol (molecular weight 200-8000), polypropylene glycol (molecular weight 400-2000), the TriMethylolPropane(TMP) polyethers (molecular weight 400-4000).
Described filler particles is to have in the ceramic particle of perovskite crystal structure one or more.Described filler particles can be BaTiO
3, PbTiO
3, PbZrO
3, Pb (Zr
1-xTi
x) O
3(0＜x＜1), Pb (Mg
1/3Nb
2/3) TiO
3-PbTiO
3, Pb (Zn
1/3Nb
2/3) TiO
3-PbTiO
3, (Ba
ySr
1-y) TiO
3(0＜y＜1), CaCu
3Ti
4O
12In a kind of or their arbitrary combination.
The present invention has also proposed a kind of method for preparing above-mentioned epoxy group(ing) composite dielectric material on the other hand.Concrete steps are: the anhydride curing agent that will contain polyether glycol graft modification agent and curing catalyst is dissolved in the organic solvent (adopting in the present embodiment acetone or butanone); Add Resins, epoxy; Add filler particles, obtain the dielectric medium slurry; Make the moulding of described dielectric medium slurry; Heating makes described solvent evaporation and solidifies.
Wherein, the material of above-mentioned polyether glycol graft modification agent, curing catalyst, anhydride curing agent, Resins, epoxy and filler particles is selected all to introduce in detail hereinbefore, does not repeat them here.
In an embodiment of the present invention, adopt five kinds of (numbering 1 to 5) components by weight percent proportionings as shown in Figure 1 to prepare described epoxy group(ing) composite dielectric material, record its specific inductivity under the 1KHZ frequency.
For contrasting effect of the present invention, adopt five kinds of (numbering 6 to 10) components by weight percent proportionings as shown in Figure 2 to prepare described epoxy group(ing) composite dielectric material conduct and contrast, record equally its specific inductivity under the 1KHZ frequency.
Figure 10 shows that employing scheme under the 1KHZ frequency (numbering 1 to 5) and scheme (numbering 6 to 10) are at different B aTiO
3The dielectric constant values contrast of the epoxy group(ing) composite dielectric material under the weight.
Can be found out by above-mentioned experimental result, epoxy group(ing) composite dielectric material that the present invention proposes and preparation method thereof is by adding described polyether glycol graft modification agent, increased the polar group content of epoxy matrix, improve the matrix polarizability, thereby improved the dielectric properties of described epoxy group(ing) composite dielectric material.
For further embodying contrast effect, under different frequency, test, experimental result such as Fig. 6 are to shown in Figure 9.Wherein, Figure 6 shows that the specific inductivity curve of electric capacity under different frequency that the epoxy group(ing) composite dielectric material that adopts five kinds mentioned above (numbering 1 to 5) components by weight percent proportionings to prepare is made; Figure 7 shows that the dielectric loss curve of electric capacity under different frequency that the epoxy group(ing) composite dielectric material that adopts described five kinds (numbering 1 to 5) components by weight percent proportionings to prepare is made; Figure 8 shows that the specific inductivity curve of electric capacity under different frequency that the epoxy group(ing) composite dielectric material that adopts five kinds mentioned above (numbering 6 to 10) components by weight percent proportionings to prepare is made; Figure 9 shows that the dielectric loss curve of electric capacity under different frequency that the epoxy group(ing) composite dielectric material that adopts described five kinds (numbering 6 to 10) components by weight percent proportionings to prepare is made.
In addition, described its specific inductivity of epoxy group(ing) composite dielectric material that employing components by weight percent proportioning as shown in Figure 3-Figure 5 prepares has preferably dielectric properties all more than 20.The specific inductivity curve of electric capacity under different frequency that Figure 11 makes for the epoxy group(ing) composite dielectric material that adopts components by weight percent proportioning shown in Figure 3 to prepare; The dielectric loss curve of electric capacity under different frequency that Figure 12 makes for the epoxy group(ing) composite dielectric material that adopts components by weight percent proportioning shown in Figure 3 to prepare; The specific inductivity curve of electric capacity under different frequency that Figure 13 makes for the epoxy group(ing) composite dielectric material that adopts components by weight percent proportioning shown in Figure 5 to prepare; The dielectric loss curve of electric capacity under different frequency that Figure 14 makes for the epoxy group(ing) composite dielectric material that adopts components by weight percent proportioning shown in Figure 5 to prepare.
Although the present invention is described with reference to current preferred embodiments; but those skilled in the art will be understood that; above-mentioned preferred embodiments only is used for illustrating the present invention; be not to limit protection scope of the present invention; any within the spirit and principles in the present invention scope; any modification of doing, equivalence replacement, improvement etc. all should be included within the scope of the present invention.
Claims (8)
1. an epoxy group(ing) composite dielectric material is characterized in that, comprises (by weight component):
100 parts of Resins, epoxy;
Anhydride curing agent 40-120 part;
Curing catalyst 1-10 part;
Polyether glycol graft modification agent 10-30 part;
Filler particles 100-400 part.
2. epoxy group(ing) composite dielectric material according to claim 1, described Resins, epoxy is selected from bisphenol A type epoxy resin, bisphenol f type epoxy resin, novolac epoxy, a kind of in the cycloaliphatic epoxy resin or their arbitrary combination, described anhydride curing agent is selected from Tetra hydro Phthalic anhydride, Tetra Hydro Phthalic Anhydride or its substitutive derivative, hexahydrophthalic anhydride or its substitutive derivative, a kind of in the Pyroglutaric acid or their arbitrary combination, described curing catalyst is selected from a kind of in methyl ethyl diketone salt or the acetoacetic ester, described polyether glycol graft modification agent is the oligopolymer of polyhydroxy-alcohol, and described filler particles is to have in the ceramic particle of perovskite crystal structure one or more.
3. epoxy group(ing) composite dielectric material according to claim 1 and 2, wherein, described polyether glycol graft modification agent is selected from a kind of in polyoxyethylene glycol, polypropylene glycol, the TriMethylolPropane(TMP) polyethers.
4. epoxy group(ing) composite dielectric material according to claim 1 and 2, wherein, described filler particles is selected from BaTiO
3, PbTiO
3, PbZrO
3, Pb (Zr
1-xTi
x) O
3, Pb (Mg
1/3Nb
2/3) TiO
3-PbTiO
3, Pb (Zn
1/3Nb
2/3) TiO
3-PbTiO
3, (Ba
ySr
1-y) TiO
3, CaCu
3Ti
4O
12In a kind of or their arbitrary combination, wherein, 0＜x＜1,0＜y＜1.
5. the preparation method of an epoxy group(ing) composite dielectric material is characterized in that, may further comprise the steps:
The anhydride curing agent that will contain polyether glycol graft modification agent and curing catalyst is dissolved in the organic solvent;
Add Resins, epoxy;
Add filler particles, obtain the dielectric medium slurry;
Make the moulding of described dielectric medium slurry;
Heating makes described solvent evaporation and solidifies.
6. the preparation method of epoxy group(ing) composite dielectric material according to claim 5, described Resins, epoxy is selected from bisphenol A type epoxy resin, bisphenol f type epoxy resin, novolac epoxy, a kind of in the cycloaliphatic epoxy resin or their arbitrary combination, described anhydride curing agent is selected from Tetra hydro Phthalic anhydride, Tetra Hydro Phthalic Anhydride or its substitutive derivative, hexahydrophthalic anhydride or its substitutive derivative, a kind of in the Pyroglutaric acid or their arbitrary combination, described curing catalyst is selected from a kind of in methyl ethyl diketone salt or the acetoacetic ester, described polyether glycol graft modification agent is the oligopolymer of polyhydroxy-alcohol, and described filler particles is to have in the ceramic particle of perovskite crystal structure one or more.
7. according to claim 5 or the preparation method of 6 described epoxy group(ing) composite dielectric materials, wherein, described polyether glycol graft modification agent is selected from a kind of in polyoxyethylene glycol, polypropylene glycol, the TriMethylolPropane(TMP) polyethers.
8. according to claim 5 or the preparation method of 6 described epoxy group(ing) composite dielectric materials, wherein, described filler particles is selected from BaTiO
3, PbTiO
3, PbZrO
3, Pb (Zr
1-xTi
x) O
3, Pb (Mg
1/3Nb
2/3) TiO
3-PbTiO
3, Pb (Zn
1/3Nb
2/3) TiO
3-PbTiO
3, (Ba
ySr
1-y) TiO
3, CaCu
3Ti
4O
12In a kind of or their arbitrary combination, wherein, 0＜x＜1,0＜y＜1.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2016029666A1 (en) * | 2014-08-29 | 2016-03-03 | 天津德高化成新材料股份有限公司 | Dielectric composite material for fingerprint sensor induction layer and preparation method therefor |
| CN114539716B (en) * | 2022-01-20 | 2023-05-09 | 国网河北省电力有限公司电力科学研究院 | Epoxy composite dielectric material and preparation method thereof |
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| CN101221832A (en) * | 2007-12-26 | 2008-07-16 | 中国科学院电工研究所 | Composite insulating material and method for producing the same |
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Application publication date: 20130424 |