RAFT聚合制备有机/无机杂化材料及其性能表征
摘要
自由基聚合所适用的单体广泛,反应条件温和,这些特点决定了其在工业生产中的主导地位,约有70%以上的塑料源于自由基聚合。但传统引发剂的慢引发、快增长、速终止等特点,导致聚合物分子量和结构的不可控。因此,活性自由基聚合的研究与开发引起了高分子学术界和工业界的高度重视及浓厚兴趣。1998年Rizzardo研究小组率先报道了他的最新研究成果RAFT活性自由基聚合,它通过在聚合体系中引进可逆加成.断裂链转移剂(如S=C(Z)S-R),使其与初级自由基和增长自由基反应形成不稳定的自由基中间体,自由基中间体可以分解产生其反应物,或者分解形成暂时失活的休眠聚合物,同时产生R自由基。自由基R可以再引发单体进行聚合。通过活性种和休眠种之间的转换,从而可以控制聚合体系中增长自由基的浓度,使聚合达到可控的目的。
1984年,Schmidt等人首先提出了有机无机材料的概念,有机无机杂化材料是一种均匀的多相材料。由于该材料综合了有机无机各自的优点,具有较高的稳定性,在阻燃性、热稳定性、机械性能等方面具有许多优异性能,因而成为材料学科研究的热点。近年来,该研究已成为高分子化学和物理、物理化学和材料科学等多门学科交叉的前沿领域,受到各国科学家的重视。
本研究论文从以下四个方面进行研究:将不同的链转移剂负载于不同的无机粒子表面,以此为链转移剂在无机粒子表面接枝聚合物;将偶氮类引发剂负载于无机粒子表面,以此为引发剂在有机链转移剂存在的情况下制备无机粒子表面接枝的嵌段聚合物;将乙烯基功能基团引入无机粒子表面,在链转移剂存在的情况下制备无机粒子表面接枝的无规共聚物;在层状硅酸盐和链转移剂存在的条件下,制备插层型有机/无机杂化材料。并利用TG-DTA、XRD、XPS、TEM、SPM、AFM、FT-IR、GPC等技术对复合材料进行了全面的表征。总体来看,用四种方法所得到的复合物分子量和结构可控,有良好的热性能。主要研究结果如下:
一、以功能化的无机粒子为链转移剂的RAFT聚合
1.研究了用乙基黄原酸基团进行表面修饰的单晶硅片作为链转移剂,通过RAFT聚合的方法制备了聚甲基丙烯酸甲酯/硅片杂化材料。结果表明PMMA已接枝到硅片表面,GPC的测试结果说明数均分子量与单体转化率呈线性关系,PDI值为1.36～1.41。
2.通过在无机材料—凹凸棒表面引入RAFT试剂,将其作为RAFT试剂,在传统的引发体系中,引发MMA聚合。XPS和FT-IR的分析结果表明,凹凸棒表面负载了RAFT试剂,PMMA已经在凹凸棒表面接枝。GPC的测试结果表明聚合反应有“活性”聚合的特征。SPM和TGA的分析结果表明,凹凸棒表面PMMA的接枝密度较高。
3.乙基黄原酸基团被成功的引到纳米二氧化硅和硅胶表面,并通过RAFT聚合将PMMA接枝到两种无机粒子的表面。聚合物的分子量、分子量分布和杂化材料的表面特征分别由GPC和SPM测得。GPC的分析结果证明这是一个“活性”/可控聚合;SPM的观测结果显示接枝到纳米二氧化硅和硅胶表面的PMMA的厚度大约分别为33.76 nm和34.02 nm。
4.通过在膨润土表面引入乙基黄原酸基团,以其为链转移剂对MMA进行了RAFT自由基聚合,制备了一种新型有机/无机纳米杂化材料,FT-IR和SPM分析结果表明,MMA已经接枝到膨润土表面。热失重分析说明,材料有良好的热稳定性,聚合物百分含量随反应时间的延长而增加,最大可达12.7%。通过凝胶色谱分析可知,所得聚合物的分子量分布很窄,单体转化率和数均分子量呈线性关系,反应在动力学上对单体浓度是一级关系说明体系中自由基浓度保持不变。
以上研究均未见国内外文献报道。
二、RAFT调控的无机粒子表面引发单体嵌段共聚合的研究
1.本文首次对埃洛石表面引发可逆加成-断裂链转移自由基聚合反应进行了研究。结果发现,聚合过程是一个“活性”/可控自由基聚合历程。分子量与单体转化率呈线性关系,ln([M]_0/[M])与反应时间成正比,二者呈线性关系,所得的杂化材料可以再次引发其它单体聚合,进一步合成了嵌段聚合物/无机纳米复合材料;热分析数据证实了杂化材料的热稳定性良好。
2.通过在纳米二氧化硅表面引入偶氮基团,以其为引发剂在离子液体中对MMA进行了RAFT自由基聚合,制备了一种有机/无机纳米杂化材料,并以此杂化材料为链转移剂再次引发了苯乙烯单体的聚合。FT-IR、~1HNMR以及元素分析表明已经成功制备了离子液体;SPM从杂化材料的外部形貌上直观的说明了PMMA在纳米二氧化硅表面的接枝情况。凝胶色谱分析可知,所得聚合物的分子量分布很窄,单体转化率和数均分子量呈线性关系,反应在动力学上对单体浓度是一级关系,符合“活性”聚合的特征。
三、RAFT调控的无规共聚物/无机纳米粒子杂化材料的制备及表征
1.本文首次通过在纳米二氧化硅表面引入乙烯基功能基团,在TNPBE链转移剂存在的情况下研究了马来酸酐与苯乙烯在纳米二氧化硅表面的接枝共聚合。实验结果表明,已成功制得了顺丁烯二酸酐和苯乙烯共聚物/纳米SiO_2复合材料杂化材料,聚合过程按照RAFT聚合机理进行。纳米SiO_2的引入,改善了材料的热性能。
2.以AIBN为引发剂,甲基丙烯酸叔丁酯基二硫代萘甲酸酯(TNPBE)为链转移剂,在有机膨润土存在的情况下进行了苯乙烯、丙烯腈的本体共聚合,其聚合行为显示活性自由基聚合特征;对材料的结构分析显示聚合物链的末端存在链转移剂的片段,苯乙烯-丙烯腈共聚物已经插入膨润土层间,对其进行的热性能测试则表明材料的热稳定性良好。
Radical polymerization is very important in industry production because it is suit to various monomers and its reaction condition is moderal. About 70% plastic come from radical polymerization. However, the traditional radical polymerization to graft the polymer chains from the substrates is difficult to control the molecular weight, molecular weight distribution as well as architectures because its slow initiation, rapid increasing and the quick terminate characteristic etc, which bring the interest of the academe and the industry of polymer in " living" polymerization. In 1998, Rizzardo reported their pioneering work RAFT polymerization. The appearance of RAFT "living" polymerization technique conquers these limitations by introducing the suitable addition-fragmentation chain transfer agents [such as S=C (Z) S-R] to the polymerization system. The system involve a reversible chain transfer in which a dithioester behaves as a transfer agent reacting with initiating and propagating radicals to give a transfer agent and a species that is able to initiate polymerization. The dithioester is transferred between the active and dormant chains, thus maintaining the living character of the polymerization.
In 1984, Schmidt etc bring forward the conception of organic/ inorganic hybrid material firstly. Organic/ inorganic hybrid material is a kind of even and multiphase material. It have become a focus of material science study because it integrate the excellence of organic and inorganic material. Polymer nanocomposites prepared by using layered materials are expected to lead to a high degree of polymer ordering and exhibit advanced gas barrier, thermal stability and enhanced mechanical properties compared to pristine polymers. In recent years, this study has become a foreland field of polymer chemistry and physics, physical chemistry and material science etc and take attention of the scientist in various country.
Four aspects are studied in this paper: polymers were grafted to the inorganic particles surface using different inorganic particles carried different CTAs as CTAs; Block copolymers were grafted to the inorganic particles surface using different inorganic particles carried azo-initiator as initiator with CTA exist; Random copolymers were grafted to the inorganic particles surface with the functional ethylene introduced onto the inorganic particles surface and CTA existed; Intercalative organic/ inorganic hybrid materials were prepared under the samdwich silicate and CTA exist. The microstructures, thermal characteristics, the organic content, the molecular weight and the molecular weight distribution of the material were characterized and measured with FT-IR, NMR, SPM, TG, GPC etc. respectively. As a whole, the complex materials prepared by this four methods own contolled molecular weight, architectures were and excellent thermal stability.The main study results as follows:
一、RAFT polymerization using functional inorganic particles as CTA
1. Si-g- PMMA polymer brushes prepared via RAFT process using modified silicon wafer as a RAFT agent are well investigated. The data obtained indicates that the PMMA are grafted on the silicon surface. The GPC analysis reveals that the Mn of the grafted polymer approximately increases linearly with increasing monomer conversion, and the polydipersity ranges (Mw/Mn) from 1.36 to 1.41.
2. This study reports a method to prepare new controlled molecular weight and low polydispity organic/"inorganic" hybrid. The XPS and FT-IR analysis indicate that the RAFT agent have been introduced onto the palygorskite surface and the PMMA have been "grafted from" the modified palygorskite. The GPC results show the RAFT polymerization is a controlled/"living" polymerization. SPM and TGA results show the organic content of the materials is high.
3. The ethyl xanthate groups have been successfully introduced to the surface of silica and silica gel. PMMA chain has grafted from the surface by RAFT polymerization using ethyl xanthate groups immobilized on silica and silica gel as surface chain transfer agent. The molecular weights, molecular weight distribution and surface properties are measured by GPC and SPM measurements. The GPC results reveal that the polymerization is a controlled process with a "living" characteristic. The SPM images show that the polymers grafted from silica and silica gel surface is uniform. The thickness of PMMA layer reaches about 34.02 nm and 33.76 nm under the RAFT polymerization condition.
4. A new type of organic/inorganic nano hybrid material are prepared though RAFT polymerization of MMA using the ethyl xanthate-terminated bentonite as CTA. FT-IR and SPM results indicate that the MMA have grafted to the bentonite surface. TG datas show the thermal stability is well, organic content of the materials is increasing with the reaction time increased which can reach 12.7 % at most. The GPC results reveal the molecular weight distribution is narrow, the Mn of the grafted polymer approximately increases linearly with increasing monomer conversion. The linear first order kinetic plot indicated that the radical concentration was constant throughout the polymerization.
These studies are not found in any other articles of the world at present.
二、The study of inorganic particles suface initiat monomer block copolymerization via RAFT.
1. Halloysite suface initiated RAFT radical polymerzaion is studied at first. The results show the polymerization is a controlled/"living" polymerization. The Mn of the grafted polymer approximately increases linearly with increasing monomer conversion and the kinetic plot is in first order. The hybrid marerial can initiate other monomer polymerization again and then block copolymer/inorganic complexes were synthesized. TG data show the materials have excellent thermal stability.
2. A kind of organic/inorganic nano hybrid material are prepared though RAFT polymerization of MMA using nano-silicon carried azo-initiator as initiator in ionic liquid. The hybrid marerial can initiate styrene monomer polymerization again. The FT-IR, ~1HNMR and elemental analysis results indicate that the ionic liquid have been successfully synthesized; SPM show that the PMMA have grafted on nano silicon surface. GPC result reveal that the molecular weight distribution is narrow, the Mn of the grafted polymer approximately increases linearly with increasing monomer conversion and the kinetic plot is in first order. The RAFT polymerization is a controlled/"living" polymerization.
三、Preparation and properties of random copolymer/inorganic nano hybrid material via RAFT.
1. MAn and St are copolymeried on silicon surface with the functional ethylene introduced onto the silicon particles surface and TNPBE existed is reported at first here. The results show the PMAn/PS/SiO2 have been preparaed successfully. The polymerization process are carried out according to RAFT mechanism. The materials' thermal stability increased because of the introduce of SiO2.
2. St and An are copolymeried using AIBN as initiator, TNPBE as CTA and the OMMT exist. The polymerization show a "living" radical polymerization characteristic. The terminal of the polymer chains have CTA segment according to the structure analysis of the material. PS/PAn copolymer have Intercalated into the layers of MMT. TG results show the material have excellent thermal stability.
1984年,Schmidt等人首先提出了有机无机材料的概念,有机无机杂化材料是一种均匀的多相材料。由于该材料综合了有机无机各自的优点,具有较高的稳定性,在阻燃性、热稳定性、机械性能等方面具有许多优异性能,因而成为材料学科研究的热点。近年来,该研究已成为高分子化学和物理、物理化学和材料科学等多门学科交叉的前沿领域,受到各国科学家的重视。
本研究论文从以下四个方面进行研究:将不同的链转移剂负载于不同的无机粒子表面,以此为链转移剂在无机粒子表面接枝聚合物;将偶氮类引发剂负载于无机粒子表面,以此为引发剂在有机链转移剂存在的情况下制备无机粒子表面接枝的嵌段聚合物;将乙烯基功能基团引入无机粒子表面,在链转移剂存在的情况下制备无机粒子表面接枝的无规共聚物;在层状硅酸盐和链转移剂存在的条件下,制备插层型有机/无机杂化材料。并利用TG-DTA、XRD、XPS、TEM、SPM、AFM、FT-IR、GPC等技术对复合材料进行了全面的表征。总体来看,用四种方法所得到的复合物分子量和结构可控,有良好的热性能。主要研究结果如下:
一、以功能化的无机粒子为链转移剂的RAFT聚合
1.研究了用乙基黄原酸基团进行表面修饰的单晶硅片作为链转移剂,通过RAFT聚合的方法制备了聚甲基丙烯酸甲酯/硅片杂化材料。结果表明PMMA已接枝到硅片表面,GPC的测试结果说明数均分子量与单体转化率呈线性关系,PDI值为1.36～1.41。
2.通过在无机材料—凹凸棒表面引入RAFT试剂,将其作为RAFT试剂,在传统的引发体系中,引发MMA聚合。XPS和FT-IR的分析结果表明,凹凸棒表面负载了RAFT试剂,PMMA已经在凹凸棒表面接枝。GPC的测试结果表明聚合反应有“活性”聚合的特征。SPM和TGA的分析结果表明,凹凸棒表面PMMA的接枝密度较高。
3.乙基黄原酸基团被成功的引到纳米二氧化硅和硅胶表面,并通过RAFT聚合将PMMA接枝到两种无机粒子的表面。聚合物的分子量、分子量分布和杂化材料的表面特征分别由GPC和SPM测得。GPC的分析结果证明这是一个“活性”/可控聚合;SPM的观测结果显示接枝到纳米二氧化硅和硅胶表面的PMMA的厚度大约分别为33.76 nm和34.02 nm。
4.通过在膨润土表面引入乙基黄原酸基团,以其为链转移剂对MMA进行了RAFT自由基聚合,制备了一种新型有机/无机纳米杂化材料,FT-IR和SPM分析结果表明,MMA已经接枝到膨润土表面。热失重分析说明,材料有良好的热稳定性,聚合物百分含量随反应时间的延长而增加,最大可达12.7%。通过凝胶色谱分析可知,所得聚合物的分子量分布很窄,单体转化率和数均分子量呈线性关系,反应在动力学上对单体浓度是一级关系说明体系中自由基浓度保持不变。
以上研究均未见国内外文献报道。
二、RAFT调控的无机粒子表面引发单体嵌段共聚合的研究
1.本文首次对埃洛石表面引发可逆加成-断裂链转移自由基聚合反应进行了研究。结果发现,聚合过程是一个“活性”/可控自由基聚合历程。分子量与单体转化率呈线性关系,ln([M]_0/[M])与反应时间成正比,二者呈线性关系,所得的杂化材料可以再次引发其它单体聚合,进一步合成了嵌段聚合物/无机纳米复合材料;热分析数据证实了杂化材料的热稳定性良好。
2.通过在纳米二氧化硅表面引入偶氮基团,以其为引发剂在离子液体中对MMA进行了RAFT自由基聚合,制备了一种有机/无机纳米杂化材料,并以此杂化材料为链转移剂再次引发了苯乙烯单体的聚合。FT-IR、~1HNMR以及元素分析表明已经成功制备了离子液体;SPM从杂化材料的外部形貌上直观的说明了PMMA在纳米二氧化硅表面的接枝情况。凝胶色谱分析可知,所得聚合物的分子量分布很窄,单体转化率和数均分子量呈线性关系,反应在动力学上对单体浓度是一级关系,符合“活性”聚合的特征。
三、RAFT调控的无规共聚物/无机纳米粒子杂化材料的制备及表征
1.本文首次通过在纳米二氧化硅表面引入乙烯基功能基团,在TNPBE链转移剂存在的情况下研究了马来酸酐与苯乙烯在纳米二氧化硅表面的接枝共聚合。实验结果表明,已成功制得了顺丁烯二酸酐和苯乙烯共聚物/纳米SiO_2复合材料杂化材料,聚合过程按照RAFT聚合机理进行。纳米SiO_2的引入,改善了材料的热性能。
2.以AIBN为引发剂,甲基丙烯酸叔丁酯基二硫代萘甲酸酯(TNPBE)为链转移剂,在有机膨润土存在的情况下进行了苯乙烯、丙烯腈的本体共聚合,其聚合行为显示活性自由基聚合特征;对材料的结构分析显示聚合物链的末端存在链转移剂的片段,苯乙烯-丙烯腈共聚物已经插入膨润土层间,对其进行的热性能测试则表明材料的热稳定性良好。
Radical polymerization is very important in industry production because it is suit to various monomers and its reaction condition is moderal. About 70% plastic come from radical polymerization. However, the traditional radical polymerization to graft the polymer chains from the substrates is difficult to control the molecular weight, molecular weight distribution as well as architectures because its slow initiation, rapid increasing and the quick terminate characteristic etc, which bring the interest of the academe and the industry of polymer in " living" polymerization. In 1998, Rizzardo reported their pioneering work RAFT polymerization. The appearance of RAFT "living" polymerization technique conquers these limitations by introducing the suitable addition-fragmentation chain transfer agents [such as S=C (Z) S-R] to the polymerization system. The system involve a reversible chain transfer in which a dithioester behaves as a transfer agent reacting with initiating and propagating radicals to give a transfer agent and a species that is able to initiate polymerization. The dithioester is transferred between the active and dormant chains, thus maintaining the living character of the polymerization.
In 1984, Schmidt etc bring forward the conception of organic/ inorganic hybrid material firstly. Organic/ inorganic hybrid material is a kind of even and multiphase material. It have become a focus of material science study because it integrate the excellence of organic and inorganic material. Polymer nanocomposites prepared by using layered materials are expected to lead to a high degree of polymer ordering and exhibit advanced gas barrier, thermal stability and enhanced mechanical properties compared to pristine polymers. In recent years, this study has become a foreland field of polymer chemistry and physics, physical chemistry and material science etc and take attention of the scientist in various country.
Four aspects are studied in this paper: polymers were grafted to the inorganic particles surface using different inorganic particles carried different CTAs as CTAs; Block copolymers were grafted to the inorganic particles surface using different inorganic particles carried azo-initiator as initiator with CTA exist; Random copolymers were grafted to the inorganic particles surface with the functional ethylene introduced onto the inorganic particles surface and CTA existed; Intercalative organic/ inorganic hybrid materials were prepared under the samdwich silicate and CTA exist. The microstructures, thermal characteristics, the organic content, the molecular weight and the molecular weight distribution of the material were characterized and measured with FT-IR, NMR, SPM, TG, GPC etc. respectively. As a whole, the complex materials prepared by this four methods own contolled molecular weight, architectures were and excellent thermal stability.The main study results as follows:
一、RAFT polymerization using functional inorganic particles as CTA
1. Si-g- PMMA polymer brushes prepared via RAFT process using modified silicon wafer as a RAFT agent are well investigated. The data obtained indicates that the PMMA are grafted on the silicon surface. The GPC analysis reveals that the Mn of the grafted polymer approximately increases linearly with increasing monomer conversion, and the polydipersity ranges (Mw/Mn) from 1.36 to 1.41.
2. This study reports a method to prepare new controlled molecular weight and low polydispity organic/"inorganic" hybrid. The XPS and FT-IR analysis indicate that the RAFT agent have been introduced onto the palygorskite surface and the PMMA have been "grafted from" the modified palygorskite. The GPC results show the RAFT polymerization is a controlled/"living" polymerization. SPM and TGA results show the organic content of the materials is high.
3. The ethyl xanthate groups have been successfully introduced to the surface of silica and silica gel. PMMA chain has grafted from the surface by RAFT polymerization using ethyl xanthate groups immobilized on silica and silica gel as surface chain transfer agent. The molecular weights, molecular weight distribution and surface properties are measured by GPC and SPM measurements. The GPC results reveal that the polymerization is a controlled process with a "living" characteristic. The SPM images show that the polymers grafted from silica and silica gel surface is uniform. The thickness of PMMA layer reaches about 34.02 nm and 33.76 nm under the RAFT polymerization condition.
4. A new type of organic/inorganic nano hybrid material are prepared though RAFT polymerization of MMA using the ethyl xanthate-terminated bentonite as CTA. FT-IR and SPM results indicate that the MMA have grafted to the bentonite surface. TG datas show the thermal stability is well, organic content of the materials is increasing with the reaction time increased which can reach 12.7 % at most. The GPC results reveal the molecular weight distribution is narrow, the Mn of the grafted polymer approximately increases linearly with increasing monomer conversion. The linear first order kinetic plot indicated that the radical concentration was constant throughout the polymerization.
These studies are not found in any other articles of the world at present.
二、The study of inorganic particles suface initiat monomer block copolymerization via RAFT.
1. Halloysite suface initiated RAFT radical polymerzaion is studied at first. The results show the polymerization is a controlled/"living" polymerization. The Mn of the grafted polymer approximately increases linearly with increasing monomer conversion and the kinetic plot is in first order. The hybrid marerial can initiate other monomer polymerization again and then block copolymer/inorganic complexes were synthesized. TG data show the materials have excellent thermal stability.
2. A kind of organic/inorganic nano hybrid material are prepared though RAFT polymerization of MMA using nano-silicon carried azo-initiator as initiator in ionic liquid. The hybrid marerial can initiate styrene monomer polymerization again. The FT-IR, ~1HNMR and elemental analysis results indicate that the ionic liquid have been successfully synthesized; SPM show that the PMMA have grafted on nano silicon surface. GPC result reveal that the molecular weight distribution is narrow, the Mn of the grafted polymer approximately increases linearly with increasing monomer conversion and the kinetic plot is in first order. The RAFT polymerization is a controlled/"living" polymerization.
三、Preparation and properties of random copolymer/inorganic nano hybrid material via RAFT.
1. MAn and St are copolymeried on silicon surface with the functional ethylene introduced onto the silicon particles surface and TNPBE existed is reported at first here. The results show the PMAn/PS/SiO2 have been preparaed successfully. The polymerization process are carried out according to RAFT mechanism. The materials' thermal stability increased because of the introduce of SiO2.
2. St and An are copolymeried using AIBN as initiator, TNPBE as CTA and the OMMT exist. The polymerization show a "living" radical polymerization characteristic. The terminal of the polymer chains have CTA segment according to the structure analysis of the material. PS/PAn copolymer have Intercalated into the layers of MMT. TG results show the material have excellent thermal stability.
引文
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69.Vana P.T.P,Barner-Kowollik C,Storing free radials using the reversible additionfragmentation chain transfer(RAFT)process,Polym.Prepr.,43,2002,321-322.
70.Barner-Kowollik C,Coote M.L,Dvis T.P,RadomL,Vana P,The ReversibleAddition-Fragmentation Chain Transfer Process and the Strength and Limitation ofModeling:Comment on "The Magnitude of the Fragmentation Rate Coeffiient,J.Polym.Chem.Part A:Polym.Chem,41,2003,2828-2832.
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73.Calitz F.M,Tonge M.P,Sanderson R.D,Kinetic and Electron spin ResonanceAnalysis of RAFT Polymerization of Styene,Macromolecules,36,2003,5-8.
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76.Toy A.A,Vana P,Davis T.P,Bamer-Kowollik C,Reversible AdditionFragmentation Chain Transfer(RAFT)Polymerization of Methyl Acrylate:DetailedStructural Investigation via Coupled Size Exclusion Chromatography-ElectrosprayIonization Mass Spectrometry(SEC-ESI-MS),Macromolecules,37,2004,744-751..
77.王艳君,王玉霞,袁才登,曹同玉。可逆加成-断裂链转移活性自由基聚合,高分子通报,3,2003,57-64.
78.John Chiefari,Roshan T.A.Mayadunne,Catherine L Moad,Graeme Moad,EzioRizzardo,Almar Postma,Melissa A.Skidmore,and San H.Thang,Thiocarbonylthio Compounds(Sd C(Z)S-R)in Free Radical Polymerization withReversible Addition-Fragmentation Chain Transfer(RAFT Polymerization).Effectof the Activating Group Z,Macromolecules,36,2003,2273-2283.
79.(Bill)Y.K.Chong,Julia Krstina,Tam P.T.Le,Graeme Moad,Almar Postma,Ezio Rizzardo,and San H.Thang,Thiocarbonylthio Compounds[SdC(Ph)S-R]inFree Radical Polymerization with Reversible Addition-Fragmentation ChainTransfer(RAPT Polymerization).Role of the Free-Radical Leaving Group(R)Macromolecules,36,,2003,2256-2272.
80.Stenzel M.H,Cummins L,Roberts G.E,Davis T.P,Vana P,Barner-kowollik C,Xanthate Mediated Living Polymerization of Vinyl Aetate:A Systematic Variationin MADIX/RAFT Agent Structure,Macromol.Chem.Phys.,204,2003,1160-1168.
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82.Adamy M,Herk A.M,Destarac M,Monteiro M.J,Inflluence of the ChemicalStructure of MADIX Agents on the RAFT Polymerization ofStyrene,Macromolecules,36,2003,2293-2301.
83.Yezi You,Chunyan Hong,Wenping Wang,Weiqi Lu,and Caiyuan.Pan,Preparation and Characterization of Thermally Responsive and BiodegradableBlock Copolymer Comprised of PNIPAAM and PLA by Combination of ROP andRAFT Methods,Macromolecules,37,2004,9761-9767.
84.Simon Harrisson and Thomas P.Davis,Pulsed Laser Copolymerization ofRing-Opening Cyclic Allylic Sulfide Monomers with Methyl Methacrylate andStyrene,Macromolecules,35,2002,2474-2480.
85.John F.Quinn,Leonie Barner,Christopher Barner-Kowollik,Ezio Rizzardo,andThomas P.Davis,Reversible Addition-Fragmentation Chain TransferPolymerization Initiated with Ultraviolet Radiation,Macromolecules,35,2002,7620-7627.
86.Stuart W.Prescott,Mathew J.Ballard,Ezio Rizzardo,and Robert G.Gilbert,Successful Use of RAFT Techniques in Seeded Emulsion Polymerization ofStyrene:Living Character,RAFT Agent Transport,and Rate of Polymerization,Macromolecules,35,2002,5417-5425.
87.Simon Harrisson and Thomas P.Davis,Copolymerization Behavior of7-Methylene-2-methyl-1,5-dithiacyclooctane:Reversible Cross-Propagation,Macromolecules,34,2001,3869-3876.
88.M.Laus,R.Papa,and K.Sparnacci,Controlled Radical Polymerization ofStyrene with Phosphoryl-and(Thiophosphoryl)dithioformates as RAFT Agents,Macromolecules,34,2001,7269-7275.
89.J.B.McLeary,F.M.Calitz,J.M.McKenzie,M.P.Tonge,R.D.Sanderson,andB.Klumperman,Beyond Inhibition:A 1H NMR Investigation of the Early Kineticsof RAFT-Mediated Polymerization with the Same Initiating and Leaving Groups,Macromolecules,37,2004,2383-2394.
90. Michael S. Donovan, Brent S. Sumerlin, Andrew B. Lowe, and Charles L. McCormick, Controlled/"Living" Polymerization of Sulfobetaine Monomers Directly in Aqueous Media via RAFT, Macromolecules, 35,2002,8663-8666.
91. David B. Thomas, Anthony J. Convertine, Roger D. Hester, Andrew B. Lowe, and Charles L. McCormick,Hydrolytic Susceptibility of Dithioester Chain Transfer Agents and Implications in Aqueous RAFT Polymerizations, Macromolecules, 37, 2004,1735-1741.
92. Alexander Theis, Achim Feldermann, Nathalie Charton, Martina H. Stenzel, Thomas P. Davis, and Christopher Barner-Kowollik, Access to Chain Length Dependent Termination Rate Coefficients of Methyl Acrylate via Reversible Addition-Fragmentation Chain Transfer Polymerization, Macromolecules, 38, 2004, 1624-1627.
93. Jean-Francu ois Lutz, Dorota Neugebauer, and Krzysztof Matyjaszewski, Stereoblock Copolymers and Tacticity Control in Controlled/Living Radical Polymerization, J. AM. CHEM. SOC. VOL. 125, NO. 23,2003,6986-6993.
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95. Michelle L. Coote and Leo Radom, Ab Initio Evidence for Slow Fragmentation in RAFT Polymerization, J. AM. CHEM. SOC. 125,2003,1490-1491.
96. Bryan Parrish and Todd Emrick, Aliphatic Polyesters with Pendant Cyclopentene Groups: Controlled Synthesis,and Conversion to Polyester-graft-PEG Copolymers, Macromolecules, 37, 2004,5863-5865.
97. David B. Thomas, Brent S. Sumerlin, Andrew B. Lowe, and Charles L. McCormick, Conditions for Facile, Controlled RAFT Polymerization of Acrylamide in Water, Macromolecules, 36,2003,1436-1439.
98. Christopher J. Ferguson, Robert J. Hughes, inh T. T. Pham, Brian S. Hawkett, Robert G. Gilbert, Algirdas K. Serelis, andChristopher H. Such,Effective ab Initio Emulsion Polymerization under RAFT Control.Macromolecules, . 35 (25), 2002, 3-7.
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102.Jeffrey Pyun and Krzysztof Matyjaszewski,Synthesis of NanocompositeOrganic/Inorganic Hybrid Materials Using Controlled/"Living" RadicalPolymerization,Chem.Mater.,2001,13,3436-3448.
103.Brent S.Sumerlin,Andrew B.Lowe,Paul A.Stroud,Ping Zhang,Marek W.Urban,and Charles L.McCormick,Modification of Gold Surfaces withater-Soluble(Co)polymers Prepared via Aqueous ReversibleAddition-Fragmentation Chain Transfer(RAFT)Polymerization,Langmuir,19,2003,5559-5562.
104.Lianjun Shi,Toby M.Chapman,(?)and Eric J.Beckman,Poly(ethyleneglycol)-block-poly(N-vinylformamide)Copolymers Synthesized by the RAFT,Methodology,Macromolecules,36,2003,2563-2567.
105.Michael S.Donovan,Taylor A.Sanford,Andrew B.Lowe,Brent S.Sumerlin,Yoshiro Mitsukami,and Charles L.McCormick,RAFT Polymerizationof N,N-Dimethylacrylamide in Water,Macromolecules,35,2002,4570-4572.
106.Chuanbing Tang,Tomasz Kowalewski,and Krzysztof Matyjaszewski,RAFTPolymerization of Acrylonitrile and Preparation of Block Copolymers Using2-Cyanoethyl Dithiobenzoate as the Transfer Agent,Macromolecules,36,2003,8587-8589.
107.Roshan T.A.Mayadunne,Graeme Moad and Ezio Rizzardo,Multiarm organic compounds for use as reversible chain-transfer,agents in living radical
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109.San H.Thang,(Bill)Y.K.Chong,Roshan T.A.Mayadunne,Graeme Moad andEzio Rizzardo,A Novel Synthesis of Functional Dithioesters,Dithiocarbamates,Xanthates and Trithiocarbonates,Tetrahedron Letters,40,1999,2435-2438.
110.Roshan T.A.Mayadunne,Justine Jeffery,Graeme Moad,and Ezio Rizzardo,Living Free Radical Polymerization with Reversible Addition-Fragmentation ChainTransfer(RAFT Polymerization):Approaches to Star Polymers,Macromolecules,36,2003,1505-1513.
111.Atsushi Goto,Koichi Sato,Yoshinobu Tsujii,Takeshi Fukuda,Graeme Moad,Ezio Rizzardo,and San H.Thang,Mechanism and Kinetics of RAFT-Based LivingRadical Polymerizations of Styrene and Methyl Methacrylate,Macromolecules,34,2001,402-408.
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125. Brent S. Sumerlin, Michael S. Donovan, Yoshiro Mitsukami, Andrew B. Lowe, and Charles L. McCormick,Water-Soluble Polymers. 84. Controlled Polymerization in Aqueous Media of Anionic Acrylamido Monomers via RAFT,Macromolecules, 34,2001,6561-6564.
126. Ce'line Farcet, Bernadette Charleux, and Rosangela Pirri,Poly(n-butyl acrylate) Homopolymer and Poly[n-butyl acrylate-b-(n-butylacrylate-co-styrene)] Block CopolymerPrepared via Nitroxide-Mediated Living/Controlled Radical Polymerization in Miniemulsion, Macromolecules, 34,2001,3823-3826.
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136.M.Laus,R.Papa,and K.Sparnacci,Controlled Radical Polymerization ofStyrene with Phosphoryl-and(Thiophosphoryl)dithioformates as RAFT Agents,Macromolecules,34,2001,7269-7275.
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146.L.Ying,W.H.Yu,E.T.Kang,and K.G.Neoh,Functional and Surface-ActiveMembranes from Poly(vinylidene fluoride)-graft-Poly(acrylic acid)Preparedvia RAFT-Mediated Graft Copolymerization,Langlnuir,20,2004,6032-6040.
147.W.H.Yu,E.T.Kang,and K.G.Neoh,Functionalization ofHydrogen-Terminated Si(100)Substrate by Surface-Initiated RAFT Polymerizationof 4-Vinylbenzyl Chloride and Subsequent Derivatization for PhotoinducedMetallization,Ind.Eng.Chem.Res.,43,2004,5194-5202.
148.Guangqun Zhai,W.H.Yu,E.T.Kang,and K.G.Neoh,Functionalization ofHydrogen-Terminated Silicon with Polybetaine Brushes via Surface-InitiatedReversible Addition-Fragmentation Chain-Transfer(RAFT)Polymerization,Ind.Eng.Chem.Res.,43,2004,1673-1680.
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154.Marina Baum and William J.Brittain,Synthesis of Polymer Brushes on SilicateSubstrates via Reversible Addition Fragmentation Chain Transfer Technique,Macromolecules,35,2002,610-615.
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