CN1958676A - Modification type clay, composite material of novolac epoxy resin of containing the clay, and predation method - Google Patents
Modification type clay, composite material of novolac epoxy resin of containing the clay, and predation method Download PDFInfo
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- CN1958676A CN1958676A CN 200510115436 CN200510115436A CN1958676A CN 1958676 A CN1958676 A CN 1958676A CN 200510115436 CN200510115436 CN 200510115436 CN 200510115436 A CN200510115436 A CN 200510115436A CN 1958676 A CN1958676 A CN 1958676A
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Abstract
This invention relates to a method for producing modified lamellar clay and phenol formaldehyde epoxy resin composite containing the modified lamellar clay. The composite comprises phenol formaldehyde epoxy resin and modified lamellar clay, which is uniformly dispersed in phenol formaldehyde epoxy resin. The intercalary layer of lamellar clay comprises two modifiers: imidazole compound and quaternary ammonium salt. This invention also provides a method for producing substrates from this composite.
Description
Technical field
The present invention relates to a kind of nano composite material, particularly a kind of clay-novolac epoxy nano composite material and manufacture method thereof.
Background technology
After electronic packaging is meant that semiconductor integrated circuit completes, be loaded in the connecting line construction with other electronic package mutual group again, become an electronic product, to reach all processing procedures of particular design function.The major function of electronic packaging has four, is respectively that electric energy transmits (Power Distribution), signal transmits (Signal Distribution), heat abstraction (Heat Dissipation) and protection support (Protection andSupport).
It is printed circuit board (PCB) that macromolecular material is used maximum electronic packagings.The printed circuit board (PCB) of combined electrical sub-component adopts the matrix material laminated plates mostly, the printed circuit board (PCB) that outer copper foil obtains requiring through etching work procedure again.Matrix material is with a kind of structural material of reinforcing fiber (as glass fibre, carbon fiber or organic fibre etc.) with resin (thermosetting resin or thermoplastic resin) be combined into.Matrix material not only has excellent physical strength, and splendid dimensional stability is also arranged simultaneously.Printed circuit board material is to adopt glass fibre the most general, because of thermosetting resin is better than thermoplastic resin on dimensional stability and thermotolerance, so resin material is to adopt thermosetting resin, wherein again to adopt Resins, epoxy the most general at present.
And nano composite material (Nanocomposite) is the matrix material of disperse phase particle diameter between 1nm～100nm, give full play to the structural performance of molecule level, character such as, high aspect ratio little, stratiform reinforced structure, ion bond as particle diameter, reaching the lightweight target of nanocomposite LR low reinforcing material content, and have high strength, high rigidity, high heat resistance, low water absorption, the contour functional property of low air penetrability.
Before general Resins, epoxy was comprised low-stress, high thermal conductivity, high heat resistance, wet fastness, erosion resistance and electric property etc. in the desired characteristic of structure package material.Require in its character under the prerequisite of increasingly stringent, we are applied in the excellent properties that nanocomposite had on the structure package material.
At first utilizing to have promotes 2-phenylimidazole (2-PI) and clay that reticulation forms to carry out intercalation modifying, then the inorganic layer material is dispersed in the Resins, epoxy, and lure that the high molecular formation of reticular pattern occurs in the interlayer of inorganic layer material into, thus, not only can utilize nanometer to blend together effect its mechanical properties is strengthened, the required character of packaged material is significantly improved as low rate of moisture absorption, high heat resistance, excellent size stability.
U.S. Pat Pat.6548576 discloses and uses two kinds of different novolac epoxys, comprise and contain 2%～13% DGEBA and 40%～70% resol approximately, can prepare at temperature range-65 ℃～150 ℃ of Resins, epoxy that do not have the heat fading phenomenon.It utilizes two kinds of different resin ratio of regulation and control, it is reached have good thermal stability.
U.S. Pat Pat.5554670 discloses with two kinds of different solidifying agent and comprises that nano composite material that BDMA and BTFA are synthesized identical epoxy resin (DGEBA) carries out crosslinkedly, and its interlamellar spacing is greater than 10nm.
U.S. Pat Pat.5760106 discloses properties-correcting agent has five kinds in the interlayer deployment conditions of clay, and the chance of wherein disperseing to form more uniformly peel ply (exfoliated) is big more, point out also in the literary composition that dispersiveness is best, its tensile strength (tensilestrength) or tensile modulus (tensile modulus) all have performed the best.
U.S. Pat Pat.5853886 discloses and comprises that with many different solidifying agent JEFFAMINE D230, D400, D4000, T304, T3000 and T5000 (the length difference of molecular chain) prepare various Resins, epoxy-clay nanocomposites, wherein interlamellar spacing (d-spacing) maximum of being worked it out with T5000 (molecular chain is the longest).
European patent EP Pat.08446661 discloses with the ratio of epoxy resin, solidifying agent and polynite at DDP/DER331/MMT=1: 1: 0.75 o'clock, its interlamellar spacing=3.438nm, then change its ratio at 1: 3: 2.5 o'clock, interlamellar spacing=3.292nm, and interlamellar spacing is supportted to such an extent that open most after using the properties-correcting agent of long carbochain instead, and mechanical properties and glass tansition temperature also are improved simultaneously.
Its result of periodical POLYMER (42) 20015947-5952 demonstrates only needs a spot of solidifying agent MPDA can reach good dispersion, if concentration is too high, can cause intercalation (intercalated) phenomenon to increase.Find out that by XRD if the amount of MPDA is too many, can cause dispersiveness bad, interlamellar spacing is controlled by MPDA, can be by 3.45nm to 18nm.
Periodical J.APPL.POLYM.SCI. (78) 2000 808-815 point out, under the situation that adds solidifying agent BDMA 3%, 5%, 180 ℃ of curing, after 1 hour, the peak value of clay 2-10 ° of detection less than.And be catalyzer or promotor (DMBA is as coupling agent) with the N-N-dimethyl benzylamine, can determine that under XRD analysis suitable adding catalyzer can make when condition of cure is the same, reach exfoliated (exfoliated) easilier.
Summary of the invention
The objective of the invention is to utilize the organic/inorganic nano BCD hybrid technology, improve dimensional stability, stripping strength, the thermotolerance of material, reduce water-intake rate.
The invention provides a kind of modified laminated clay, comprise a stratiform clay, its intercalation has two kinds of properties-correcting agent, comprises imidazoles (imidazole) compound and quarternary ammonium salt.
The present invention provides a kind of clay-composite material of novolac epoxy resin in addition, comprises a novolac epoxy, and just like above-mentioned modified laminated clay, this modified laminated clay is dispersed in this novolac epoxy.
The present invention provides a kind of manufacture method of clay-composite material of novolac epoxy resin again, comprise the following steps: to provide modified laminated clay just like above-mentioned, mix this modified laminated clay and a solidifying agent, and an above-mentioned modified clay and a novolac epoxy that contains solidifying agent carried out crosslinking reaction, this modified clay is dispersed in this novolac epoxy, forms one clay-composite material of novolac epoxy resin.
According to the present invention, can effectively improve dimensional stability, stripping strength, thermotolerance, reduce water-intake rate.
Embodiment
The invention provides a kind of modified laminated clay, comprise a stratiform clay, its intercalation has two properties-correcting agent, comprises imidazoles (imidazole) compound and quarternary ammonium salt.
Above-mentioned two properties-correcting agent are to wait molar ratio mixing intercalation in laminated clay, and its weight percent in laminated clay is probably between 1wt%～25wt%.Imidazolium compounds can comprise glyoxal ethyline, 4-methylimidazole, 2-ethyl imidazol(e), 4-ethyl imidazol(e), 2-phenylimidazole or 4-phenylimidazole.Quarternary ammonium salt can comprise Benzene Chloride diformazan hydrocarbon ammonium (benzalkonium chloride, BKC).Laminated clay can comprise silicon aluminite class clay (smectite clay), vermiculite (vermiculite), halloysite (halloysite), sericite (sericite) or mica (mica), and smectites clay (smectite clay) can comprise polynite (montmorillonite), saponite (saponite), beidellite (beidellite), nontronite (nontronite) or lithium soap soil (hectorite).(cation exchange capacity is CEC) substantially between 50～200meq/100g for the cation exchange capacity of laminated clay of the present invention.And the interlamellar spacing of modified laminated clay is greater than 1.6nm.
The present invention provides a kind of clay-composite material of novolac epoxy resin in addition, comprises a novolac epoxy, and just like above-mentioned modified laminated clay, this modified laminated clay is dispersed in the novolac epoxy.
Novolac epoxy can comprise dihydroxyphenyl propane (bisphenol A) novolac epoxy, and its solid content is substantially between 93wt%～99.5wt%.Also comprising the intercalation solidifying agent in above-mentioned modified laminated clay, for example is resol (phenolic novolac) or tetrabromo-bisphenol (tetrabromo bisphenol A) resin, and its content is substantially between 20wt%～55wt%.In matrix material, the two weight ratio of solidifying agent and novolac epoxy is substantially between 0.20～0.55, and modified laminated clay accounts for 0.5～7 weight percent of whole matrix material substantially.
The interlamellar spacing of matrix material of the present invention is greater than 5nm.Its water-absorbent is lower than 0.6%, the Copper Foil stripping strength is greater than 1.05N/mm, glass transition temperature (glass transitiontemperature, Tg) be higher than 130 degrees centigrade, and the temperature expansion coefficient before glass transition temperature (coefficient of thermal expansion CTE) is lower than 60ppm/ ℃.
The present invention provides a kind of manufacture method of clay-composite material of novolac epoxy resin again, comprise the following steps: at first, provide just like above-mentioned modified laminated clay, then, a mixed and modified type laminated clay and a solidifying agent afterwards, carry out crosslinking reaction with an above-mentioned modified clay and a novolac epoxy that contains solidifying agent, modified clay is dispersed in the novolac epoxy, forms one clay-composite material of novolac epoxy resin.
Clay-composite material of novolac epoxy resin of the present invention also can be used for the making of copper clad laminate, comprises the following steps: at first, clay-composite material of novolac epoxy resin and glass cloth is dipped in contain in the immersion trough.Then, will contain impregnated glass is arranged in and lasts about 3～5 minutes in about 170～190 degrees centigrade baking oven of temperature and form film.Afterwards, film is cut, storehouse and hot pressing.After last cutting edge, and the copper clad laminate that contains clay-composite material of novolac epoxy resin of promptly completing (copper cladlaminate, CCL).
Below by several embodiment to further specify the features and advantages of the present invention.
Embodiment 1
The making of modified laminated clay (PK-805)
At first, in the deionized water with 2700 milliliters of 30 PK-805 clays (canbyite) addings that restrain, stirring is spent the night, and carries out swelling and handles.Simultaneously, prepare an amount of properties-correcting agent, it is dissolved fully waiting the 2-phenylimidazole (2-PI) of molar ratio to add in the appropriate amount of deionized water, stirring with Benzene Chloride diformazan hydrocarbon ammonium.Then, properties-correcting agent is slowly added above-mentioned clayish solution, wherein the properties-correcting agent weight percent that accounts for modified laminated clay is respectively 1wt%, 5wt%, 10wt%, 20wt%, 25wt% to scale, and adjusts its pH value between 3～4 with the hydrochloric acid of 1N, and stirring is spent the night.Afterwards, it is centrifugal that solution is put into centrifugal bottle, centrifugal after, the aqueous solution is abandoned, take off a layer sedimentary clays, utilize deionized water swelling, stirring again.Repeated centrifugation splashes into Silver Nitrate up to upper water solution for several times, does not have till the white precipitate of silver chloride.After lower floor's clay is put into refrigerator, put into freeze drier again and treat complete drying, promptly finish the making of modified laminated clay of the present invention.The interlamellar spacing of this modified laminated clay is 1.801nm.Wait molar ratio blended glyoxal ethyline (2-MI) and Benzene Chloride diformazan hydrocarbon ammonium if properties-correcting agent changes into, the interlamellar spacing of the modified laminated clay of then making is 1.765nm.
Embodiment 2
The making of modified laminated clay (PK-802)
At first, in the deionized water with 2700 milliliters of 30 PK-802 clays (polynite) addings that restrain, stirring is spent the night, and carries out swelling and handles.Simultaneously, prepare an amount of properties-correcting agent, it is dissolved fully waiting the 2-phenylimidazole and the Benzene Chloride diformazan hydrocarbon ammonium of molar ratio to add in the appropriate amount of deionized water, stirring.Then, properties-correcting agent is slowly added above-mentioned clayish solution, wherein the properties-correcting agent weight percent that accounts for modified laminated clay is respectively 1wt%, 5wt%, 10wt%, 20wt%, 25wt% to scale, and adjusts its pH value between 3～4 with the hydrochloric acid of 1N, and stirring is spent the night.Afterwards, it is centrifugal that solution is put into centrifugal bottle, centrifugal after, the aqueous solution is abandoned, take off a layer sedimentary clays, utilize deionized water swelling, stirring again.Repeated centrifugation splashes into Silver Nitrate up to upper water solution for several times, does not have till the white precipitate of silver chloride.After lower floor's clay is put into refrigerator, put into freeze drier again and treat complete drying, promptly finish the making of modified laminated clay of the present invention.The interlamellar spacing of this modified laminated clay is 1.714nm.Wait molar ratio blended glyoxal ethyline (2-MI) and Benzene Chloride diformazan hydrocarbon ammonium if properties-correcting agent changes into, the interlamellar spacing of the modified laminated clay of then making is 1.605nm.
Embodiment 3
The making of modified laminated clay (Kunipia-F)
At first, in the deionized water with 2700 milliliters of 30 Kunipia-F clays (polynite) addings that restrain, stirring is spent the night, and carries out swelling and handles.Simultaneously, prepare an amount of properties-correcting agent, it is dissolved fully waiting the 2-phenylimidazole and the Benzene Chloride diformazan hydrocarbon ammonium of molar ratio to add in the appropriate amount of deionized water, stirring.Then, properties-correcting agent is slowly added above-mentioned clayish solution, wherein the properties-correcting agent weight percent that accounts for modified laminated clay is respectively 1wt%, 5wt%, 10wt%, 20wt%, 25wt% to scale, and adjusts its pH value between 3～4 with the hydrochloric acid of 1N, and stirring is spent the night.Afterwards, it is centrifugal that solution is put into centrifugal bottle, centrifugal after, the aqueous solution is abandoned, take off a layer sedimentary clays, utilize deionized water swelling, stirring again.Repeated centrifugation splashes into Silver Nitrate up to upper water solution for several times, does not have till the white precipitate of silver chloride.After lower floor's clay is put into refrigerator, put into freeze drier again and treat complete drying, promptly finish the making of modified laminated clay of the present invention.The interlamellar spacing of this modified laminated clay is 1.748nm.Wait molar ratio blended glyoxal ethyline (2-MI) and Benzene Chloride diformazan hydrocarbon ammonium if properties-correcting agent changes into, the interlamellar spacing of the modified laminated clay of then making is 1.766nm.
Embodiment 4
The making of nano composite material
At first, (propylene glycol monomethyl ether stirs in solvent PM), and it is dissolved fully an amount of PK-805 modified clay to be added propylene glycol monomethyl ether.Then, an amount of solidifying agent-resol (phenolicnovolac) is added in the above-mentioned clayish solution, make itself and modified clay mixing intercalation.Afterwards, novolac epoxy (novolac epoxy) is added in the clayish solution, stir and make its homodisperse.For example, at first the modified clay with 21g adds among the PM of 420ml, and the solidifying agent-resol with 548g adds above-mentioned solution again, adds the novolac epoxy (novolac epoxy) of 500g at last again.Then, this resin solution is poured in the mould, and placed vacuum drying oven, solvent is drained.Afterwards, put into Hotaircirculatingoven, carry out material cured, solidification value is 190 degrees centigrade, lasts 90 minutes, after the taking-up, is clay-composite material of novolac epoxy resin of the present invention.
Though the present invention discloses as above with preferred embodiment, so it is not in order to limit the present invention.Those skilled in the art without departing from the spirit and scope of the present invention, can do further improvement and variation on this basis, so the scope that claims were defined that protection scope of the present invention is worked as with the application is as the criterion.
Claims (34)
1. modified laminated clay comprises:
One stratiform clay, its intercalation have two kinds of properties-correcting agent, comprise imidazolium compounds and quarternary ammonium salt.
2. modified laminated clay according to claim 1 is characterized in that, above-mentioned properties-correcting agent is to wait molar ratio to mix.
3. modified laminated clay according to claim 1 is characterized in that, this imidazolium compounds comprises glyoxal ethyline, 4-methylimidazole, 2-ethyl imidazol(e), 4-ethyl imidazol(e), 2-phenylimidazole or 4-phenylimidazole.
4. modified laminated clay according to claim 1 is characterized in that, this quarternary ammonium salt comprises Benzene Chloride diformazan hydrocarbon ammonium.
5. modified laminated clay according to claim 1 is characterized in that the per-cent of above-mentioned properties-correcting agent gross weight is between 1wt%～25wt%.
6. modified laminated clay according to claim 1 is characterized in that, this laminated clay is selected from the set that silicon aluminite class clay, vermiculite, halloysite, sericite and mica are formed.
7. modified laminated clay according to claim 6 is characterized in that, this silicon aluminite class clay is selected from the set that polynite, saponite, beidellite, nontronite and lithium soap soil are formed.
8. modified laminated clay according to claim 1 is characterized in that the cation exchange capacity of this laminated clay is between 50～200meq/100g.
9. modified laminated clay according to claim 1 is characterized in that the interlamellar spacing of this modified laminated clay is greater than 1.6nm.
10. clay-composite material of novolac epoxy resin comprises:
One novolac epoxy; And
One modified laminated clay according to claim 1, this modified laminated clay is dispersed in this novolac epoxy.
11. clay-composite material of novolac epoxy resin according to claim 10 is characterized in that, this novolac epoxy comprises bisphenol-A phenolic Resins, epoxy.
12. clay-composite material of novolac epoxy resin according to claim 10 is characterized in that, the solid content of this novolac epoxy is between 93wt%～99.5wt%.
13. clay-composite material of novolac epoxy resin according to claim 10 is characterized in that, it also comprises a solidifying agent, and intercalation is in this modified laminated clay.
14. clay-composite material of novolac epoxy resin according to claim 13 is characterized in that, this solidifying agent comprises resol or tetrabromo-bisphenol resin.
15. clay-composite material of novolac epoxy resin according to claim 13 is characterized in that, the content of this solidifying agent is between 20wt%～55wt%.
16. clay-composite material of novolac epoxy resin according to claim 13 is characterized in that, the weight ratio of this solidifying agent and this novolac epoxy is between 0.20～0.55.
17. clay-composite material of novolac epoxy resin according to claim 10 is characterized in that, the weight percent of this modified laminated clay is between 0.5wt%～7wt%.
18. clay-composite material of novolac epoxy resin according to claim 10 is characterized in that, the interlamellar spacing of this matrix material is greater than 5nm.
19. clay-composite material of novolac epoxy resin according to claim 10 is characterized in that, the water-absorbent of this matrix material is lower than 0.6%.
20. clay-composite material of novolac epoxy resin according to claim 10 is characterized in that, the Copper Foil stripping strength of this matrix material is greater than 1.05N/mm.
21. clay-composite material of novolac epoxy resin according to claim 10 is characterized in that, the glass transition temperature of this matrix material is higher than 130 degrees centigrade.
22. clay-composite material of novolac epoxy resin according to claim 21 is characterized in that, the temperature expansion coefficient of this matrix material before glass transition temperature is lower than 60ppm/ ℃.
23. the manufacture method of a clay-composite material of novolac epoxy resin, it comprises:
One modified laminated clay according to claim 1 is provided;
Mix this modified laminated clay and a solidifying agent; And
An above-mentioned modified clay and a novolac epoxy that contains solidifying agent carried out crosslinking reaction, this modified clay is dispersed in this novolac epoxy, form one clay-composite material of novolac epoxy resin.
24. the manufacture method of clay-composite material of novolac epoxy resin according to claim 23 is characterized in that, this novolac epoxy comprises bisphenol-A phenolic Resins, epoxy.
25. the manufacture method of clay-composite material of novolac epoxy resin according to claim 23 is characterized in that, the solid content of this novolac epoxy is between 93wt%～99.5wt%.
26. the manufacture method of clay-composite material of novolac epoxy resin according to claim 23 is characterized in that, this solidifying agent comprises resol or tetrabromo-bisphenol resin.
27. the manufacture method of clay-composite material of novolac epoxy resin according to claim 23 is characterized in that, the content of this solidifying agent is between 20wt%～55wt%.
28. the manufacture method of clay-composite material of novolac epoxy resin according to claim 23 is characterized in that, the weight ratio of this solidifying agent and this novolac epoxy is between 0.2～0.55.
29. the manufacture method of clay-composite material of novolac epoxy resin according to claim 23 is characterized in that, the weight percent of this modified laminated clay in this matrix material is between 0.5wt%～7wt%.
30. the manufacture method of clay-composite material of novolac epoxy resin according to claim 23 is characterized in that, the interlamellar spacing of this matrix material is greater than 5nm.
31. the manufacture method of clay-composite material of novolac epoxy resin according to claim 23 is characterized in that, the water-absorbent of this matrix material is lower than 0.6%.
32. the manufacture method of clay-composite material of novolac epoxy resin according to claim 23 is characterized in that, the Copper Foil stripping strength of this matrix material is greater than 1.05N/mm.
33. the manufacture method of clay-composite material of novolac epoxy resin according to claim 23 is characterized in that, the glass transition temperature of this matrix material is higher than 130 degrees centigrade.
34. the manufacture method of clay-composite material of novolac epoxy resin according to claim 33 is characterized in that, the temperature expansion coefficient of this matrix material before glass transition temperature is lower than 60ppm/ ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510115436 CN1958676A (en) | 2005-11-03 | 2005-11-03 | Modification type clay, composite material of novolac epoxy resin of containing the clay, and predation method |
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| CN 200510115436 CN1958676A (en) | 2005-11-03 | 2005-11-03 | Modification type clay, composite material of novolac epoxy resin of containing the clay, and predation method |
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| CN1958676A true CN1958676A (en) | 2007-05-09 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101747533B (en) * | 2008-12-04 | 2012-05-09 | 私立中原大学 | Modification clay and clay-high polymer composite |
| CN109943301A (en) * | 2019-03-28 | 2019-06-28 | 中国石油大学(华东) | Resin emulsion sealing agent composition and preparation method thereof and the application in fracture formation |
| DE102009030248B4 (en) | 2008-06-24 | 2020-07-09 | Chung Yuan Christian University | Modified clay and clay-polymer composite |
-
2005
- 2005-11-03 CN CN 200510115436 patent/CN1958676A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102009030248B4 (en) | 2008-06-24 | 2020-07-09 | Chung Yuan Christian University | Modified clay and clay-polymer composite |
| CN101747533B (en) * | 2008-12-04 | 2012-05-09 | 私立中原大学 | Modification clay and clay-high polymer composite |
| CN109943301A (en) * | 2019-03-28 | 2019-06-28 | 中国石油大学(华东) | Resin emulsion sealing agent composition and preparation method thereof and the application in fracture formation |
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Application publication date: 20070509 |