A novel unsymmetrical dianhydride containing 4\|(4\|hydroxylphenyl)\|2,3\|phthalazin\|1\|one was synthesized in order to improve the solubility of aromatic polyimides according to the principle of designing new monome...A novel unsymmetrical dianhydride containing 4\|(4\|hydroxylphenyl)\|2,3\|phthalazin\|1\|one was synthesized in order to improve the solubility of aromatic polyimides according to the principle of designing new monomers.This article reported a series of polyimide random copolymers derived from 4,4′ diamino diphenyl sulfone (DAPS),4,4′ oxyl dianiline (ODA) and the new dianhydride\|2 (3,4 dicarboxyl phenyl) 4 (3′,4′ dicarboxyl phenyl oxyl) phenyl 2,3 phthalazine 1 one dianhydride (DAH4) by“one step”solution polycondensation in m cresol with catalystic amount of isoquinoline at 200℃.Some properties of the copolymers were investigated by DSC,TG and mechanical analysis.The result shows that the η inh of copolymers is between 0 64 to 0 71 dL/g in m cresol at 25℃,and the T g of the copolymers are higher than that of pure poliymides containing 4,4′ oxyl dianiline (polymer 5).The relationship between T g and mole percent of DAPS is not obvious.Degradation temperature for 5% weight loss ( T d5 ) of the copolymers occurs all above 470℃ in air.The mechanical properties of the copolymers are lower owing to introducing sulfone groups into polymer’s backbone.In sharp contrast,the copolymers have good solubility and can be easily soluble in 1,1,2,2 tetrachloroethane(TCE), N,N dimethylacetamide(DMAc), N methyl 2 pyrrolidinone (NMP), m cresol and pyridine.Furthermore,the copolymers have better solubility in dimethyl sulfoxide (DMSO) and chloroform than the polyimide derived from DAH4 and ODA.展开更多
High-performance low-k and low-loss circuit materials are urgently needed in the field of microelectronics due to the upcoming FifthGeneration Mobile Communications Technology(5 G Technology).Herein,a facile design st...High-performance low-k and low-loss circuit materials are urgently needed in the field of microelectronics due to the upcoming FifthGeneration Mobile Communications Technology(5 G Technology).Herein,a facile design strategy for non-fluorinated intrinsic low-k and low-loss polyimides is reported by fully considering the secondary relaxation behaviors of the polymer chains.A new amorphous non-fluorinated polymer(TmBPPA)with a k value of 2.23 and a loss tangent lower than 3.94×10^-3 at 104 Hz has been designed and synthesized,which to the best of our knowledge is the lowest value amongst the non-fluorinated and non-porous polymers reported in literature.Meanwhile,TmBPPA exhibits excellent overall properties,such as excellent thermostability,good mechanical properties,low moisture absorption,and high bonding strength.As high-performance flexible circuit materials,all these characteristics are highly expected to meet the present and future demands for high density,high speed,and high frequency electronic circuit used in 5 G wireless networks.展开更多
The monomer 2,6,12-triaminotriptycene was synthesized and the structure was confirmed by IR and 1H NMR spectra. Hyperbranched polyimides modified with different terminal groups were obtained from precursors, anhydride...The monomer 2,6,12-triaminotriptycene was synthesized and the structure was confirmed by IR and 1H NMR spectra. Hyperbranched polyimides modified with different terminal groups were obtained from precursors, anhydride- and aminoterminated hyperbranched poly（amic acid）s from polymerization of A2 ＋ B3 system. From gel permeation chromatograrn （GPC） characterization, representative products had high molecular weight. All polymers had good solubility in CHCl3, DMF and tetrahydrofuran （THF）, and performed no detective Tgs in the range of 50-300 ℃ and high Tds above 455 ℃ when 5% weight loss.展开更多
A new unsymmetrical and noncoplanar diamine containing trifluoromethyl and trimethyl groups, 1,4-bis（4- amino-2-trifluoromethylphenoxy）-2,3,5-trimethylbenzene （2）, was synthesized using 2,3,5-trimethylhydroquinone...A new unsymmetrical and noncoplanar diamine containing trifluoromethyl and trimethyl groups, 1,4-bis（4- amino-2-trifluoromethylphenoxy）-2,3,5-trimethylbenzene （2）, was synthesized using 2,3,5-trimethylhydroquinone and 2-chloro-5-nitrobenzotrifluoride as starting materials. A series of fluorinated poly（ether imide）s （PEIs） （4a-4d） were prepared from diamine 2 with four aromatic dianhydrides via a one-step high-temperature polycondensation procedure. The obtained PEIs were readily soluble in most organic solvents and could be solution-cast into flexible and strong films. The resulting thin films exhibited light color and good optical transparency with a cutoff wave- length of 356--376 nm. They also displayed good thermal stability with glass transition temperatures （Tg） above 281℃, 10% weight loss temperatures in the range of 482--486 ~C, and the weight residue more than 55% at 800℃ in nitrogen. Moreover, they revealed low dielectric constants （2.77-2.93 at 1 MHz） and low moisture absorp- tions （0.41%-0.57%）.展开更多
A new aromatic diamine containing trifluoromethyl and methyl groups, namely a,a-bis（4-amino-3-methylphetayl）-4-（trifluoromethyl）phenylmethane （1）, was synthesized from 2-methylaniline and 4-（trifluoromethyl）- ...A new aromatic diamine containing trifluoromethyl and methyl groups, namely a,a-bis（4-amino-3-methylphetayl）-4-（trifluoromethyl）phenylmethane （1）, was synthesized from 2-methylaniline and 4-（trifluoromethyl）- benzaldehyde. A series of fluorinated polyimides （PIs） were prepared from the diamine with four commercially available aromatic tetracarboxylic dianhydrides using a one-step high-temperature polycondensation procedure. These obtained PIs showed excellent solubility, with the dissolvability at a concentration of 10 wt% in most solvents, and they could afford flexible and strong films. Thin films of these PIs exhibited high optical transparency and light color, with the cutoff wavelength at 324-357 nm and transmittance higher than 74% at 450 nm. Moreover, these Pls possessed eminent thermal stability and good mechanical properties.展开更多
文摘A novel unsymmetrical dianhydride containing 4\|(4\|hydroxylphenyl)\|2,3\|phthalazin\|1\|one was synthesized in order to improve the solubility of aromatic polyimides according to the principle of designing new monomers.This article reported a series of polyimide random copolymers derived from 4,4′ diamino diphenyl sulfone (DAPS),4,4′ oxyl dianiline (ODA) and the new dianhydride\|2 (3,4 dicarboxyl phenyl) 4 (3′,4′ dicarboxyl phenyl oxyl) phenyl 2,3 phthalazine 1 one dianhydride (DAH4) by“one step”solution polycondensation in m cresol with catalystic amount of isoquinoline at 200℃.Some properties of the copolymers were investigated by DSC,TG and mechanical analysis.The result shows that the η inh of copolymers is between 0 64 to 0 71 dL/g in m cresol at 25℃,and the T g of the copolymers are higher than that of pure poliymides containing 4,4′ oxyl dianiline (polymer 5).The relationship between T g and mole percent of DAPS is not obvious.Degradation temperature for 5% weight loss ( T d5 ) of the copolymers occurs all above 470℃ in air.The mechanical properties of the copolymers are lower owing to introducing sulfone groups into polymer’s backbone.In sharp contrast,the copolymers have good solubility and can be easily soluble in 1,1,2,2 tetrachloroethane(TCE), N,N dimethylacetamide(DMAc), N methyl 2 pyrrolidinone (NMP), m cresol and pyridine.Furthermore,the copolymers have better solubility in dimethyl sulfoxide (DMSO) and chloroform than the polyimide derived from DAH4 and ODA.
基金finincially supported by the National Natural Science Foundation of China (Nos. 51373204 and 51873239)the National 973 Program of China (No. 2014CB643605)+3 种基金the Science and Technology Project of Guangdong Province (Nos. 2015B090915003 and 2015B090913003)the Leading Scientific, Technical and Innovation Talents of Guangdong Special Support Program (No. 2016TX03C295)the China Postdoctoral Science Foundation (No. 2017M612801)the Fundamental Research Funds of Sun Yat-sen University
文摘High-performance low-k and low-loss circuit materials are urgently needed in the field of microelectronics due to the upcoming FifthGeneration Mobile Communications Technology(5 G Technology).Herein,a facile design strategy for non-fluorinated intrinsic low-k and low-loss polyimides is reported by fully considering the secondary relaxation behaviors of the polymer chains.A new amorphous non-fluorinated polymer(TmBPPA)with a k value of 2.23 and a loss tangent lower than 3.94×10^-3 at 104 Hz has been designed and synthesized,which to the best of our knowledge is the lowest value amongst the non-fluorinated and non-porous polymers reported in literature.Meanwhile,TmBPPA exhibits excellent overall properties,such as excellent thermostability,good mechanical properties,low moisture absorption,and high bonding strength.As high-performance flexible circuit materials,all these characteristics are highly expected to meet the present and future demands for high density,high speed,and high frequency electronic circuit used in 5 G wireless networks.
基金the National Natural Science Foundation(No.50673031)of China and authors would like to extend thanks to Professor Yongming Chen at CAS.
文摘The monomer 2,6,12-triaminotriptycene was synthesized and the structure was confirmed by IR and 1H NMR spectra. Hyperbranched polyimides modified with different terminal groups were obtained from precursors, anhydride- and aminoterminated hyperbranched poly（amic acid）s from polymerization of A2 ＋ B3 system. From gel permeation chromatograrn （GPC） characterization, representative products had high molecular weight. All polymers had good solubility in CHCl3, DMF and tetrahydrofuran （THF）, and performed no detective Tgs in the range of 50-300 ℃ and high Tds above 455 ℃ when 5% weight loss.
基金This work was supported by the National Natural Science Foundation of China （No. 51103016）, the Natural Science Foundation of Jiangsu Province （No. BK2011232 and BK2011241）, the Grant-in-aid for Youth Innovation Fundation of Changzhou University （No. ZMFll020017 and ZMFl102037）, and the Open- ing Project of State Key Laboratory for Modification of Chemical Fibers and Polymer Materials （No. LK1001）.
文摘A new unsymmetrical and noncoplanar diamine containing trifluoromethyl and trimethyl groups, 1,4-bis（4- amino-2-trifluoromethylphenoxy）-2,3,5-trimethylbenzene （2）, was synthesized using 2,3,5-trimethylhydroquinone and 2-chloro-5-nitrobenzotrifluoride as starting materials. A series of fluorinated poly（ether imide）s （PEIs） （4a-4d） were prepared from diamine 2 with four aromatic dianhydrides via a one-step high-temperature polycondensation procedure. The obtained PEIs were readily soluble in most organic solvents and could be solution-cast into flexible and strong films. The resulting thin films exhibited light color and good optical transparency with a cutoff wave- length of 356--376 nm. They also displayed good thermal stability with glass transition temperatures （Tg） above 281℃, 10% weight loss temperatures in the range of 482--486 ~C, and the weight residue more than 55% at 800℃ in nitrogen. Moreover, they revealed low dielectric constants （2.77-2.93 at 1 MHz） and low moisture absorp- tions （0.41%-0.57%）.
基金Acknowledgement This word was supported by the National Natural Science Foundation of China （No. 51103016）, Natural Science Foundation of Jiangsu Province （Nos. BK2011232 and BK2011241）, the Grant-in-aid for Youth Innovation Fundation of Changzhou University （Nos. ZMF 11020017 and ZMF 1102037）, and the Opening Project of State Key Laboratory for Modification of Chemical Fibers and Polymer Materials （No. LK1001）.
文摘A new aromatic diamine containing trifluoromethyl and methyl groups, namely a,a-bis（4-amino-3-methylphetayl）-4-（trifluoromethyl）phenylmethane （1）, was synthesized from 2-methylaniline and 4-（trifluoromethyl）- benzaldehyde. A series of fluorinated polyimides （PIs） were prepared from the diamine with four commercially available aromatic tetracarboxylic dianhydrides using a one-step high-temperature polycondensation procedure. These obtained PIs showed excellent solubility, with the dissolvability at a concentration of 10 wt% in most solvents, and they could afford flexible and strong films. Thin films of these PIs exhibited high optical transparency and light color, with the cutoff wavelength at 324-357 nm and transmittance higher than 74% at 450 nm. Moreover, these Pls possessed eminent thermal stability and good mechanical properties.
