均聚物/表面活性剂或无规共聚物的水相自组装及微反应器应用
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摘要
长期以来,胶体与界面化学家对小分子表面活性剂如何自组装成各种尺度和形貌的胶束进行了系统和深入的研究,也关注表面活性剂与水溶性均聚物的复合体系,即它们的共同自组装行为。均聚物与表面活性剂两者间的相互作用,能够改变表面活性剂的自组装行为,产生新的共同自组装体。事实上,这种复合体系已经在生命科学、药品与食品、三次采油、日用化学品、纳米材料制备等领域得到广泛应用。
研究表面活性剂与水溶性非离子均聚物的共同自组装,目前主要集中在对表面活性剂双临界浓度现象、两者间相互作用部位或其具体应用等方面,却少有对两者间自组装定量规律的研究。因此,本论文关注的第一个问题是：能否从定量层面考察均聚物与表面活性剂共同自组装行为,并探索共同自组装体的微结构和宏结构?
湿化学法是目前合成无机纳米材料的主要方法之一,其中大量使用表面活性剂或水溶性聚合物作包覆剂,目前也有一些同时使用两者作复合包覆剂的报导。但是,由于对复合包覆剂的功能不甚清楚,因而很难对目标无机纳米材料的尺度和形貌进行有效的调控。因此,本论文关注的第二个问题是：能否在深入了解水溶性非离子均聚物／表面活性剂共同自组装体微结构和宏结构的基础上,以其作为微反应器,调控其中目标金属还原产物的尺度和形貌?
双亲性无规共聚物廉价易得,较之于两亲嵌段共聚物或接枝共聚物而言更有潜在的应用价值。但双亲性无规共聚物具有“短亲/疏水链段”的链结构特点,使其不能形成类似于两亲嵌段共聚物或接枝共聚物胶束、或非共价键合胶束的明确核壳结构,因而在大分子自组装中少受关注。因此,本论文关注的第三个问题是：双亲性无规共聚物能否在完全水相环境中自组装成新的聚集构造以及用作制备金属微纳结构的微反应器的可能性?
围绕以上提出的三个问题,本论文的主要工作分为以下三个方面：
1、定量研究PVP或PEG与SDS的共同自组装
采用表面张力、电导率、超滤、增溶、荧光分子探针等研究手段,获得聚乙烯毗咯烷酮(PVP)/十二烷基硫酸钠(SDS)和聚乙二醇(PEG)/SDS复合体系水溶液中SDS的第一临界浓度c1、第二临界浓度c2和束缚胶束聚集数N等数据。研究水溶性非离子均聚物/表面活性剂的共同组装过程,得到三个主要特征参数,以其反映两者间共同自组装的边界和定量关系：(1)饱和束缚比[B],反映每个束缚胶束化SDS分子结合均聚物链节的最大能力；(2)临界束缚胶束聚集数[N],反映均聚物上形成SDS束缚胶束的最小聚集数；(3)聚合物分子量阈值[M],反映共同自组装所要求的最小聚合物分子量。实验事实表明,上述三个新特征参数都是只由表面活性剂及均聚物的分子结构确定的不变量,而受聚合物分子量([M]除外)和浓度等的影响很小。综合SDS的临界浓度、三个特征参数与核磁共振、浊点、克拉夫特点以及流变性等实验结果,证明PVP/SDS共同自组装体既具有“拟聚电解质”微结构,又具有项链状宏结构。
2、PVP/SDS共同自组装体的微反应器应用
将PVP/SDS共同自组装体作为制备金属微纳结构的微反应器,发现该微反应器的“拟聚电解质”微结构具有富集金属反离子功能,其项链状宏结构可以发挥调控金属还原产物的形貌和尺度的功能。在PVP/SDS微反应器中,借助晶体生长、微反应器调控与环境影响因素等因子之间的竞争和协同作用,合成了金、银、镍、铜等元素的准3-D、2-D、1-D乃至0-D金属微纳结构,从而在同一种微反应器中分别获得了多种成分、多种维度以及多种形貌的金属微纳结构。本研究结果表明,使用水溶性非离子均聚物/表面活性剂自组装体作微反应器,可对生成的金属微纳结构实施更有效的调控,这对推进湿化学方法制备金属微纳结构具有较大实用意义。
3、HPAM的pH响应性自组装及微反应器应用
考察部分水解聚丙烯酰胺(HPAM)在水相中的pH响应性自组装行为。在pH诱导下,HPAM在水相中能够独自组装、或经第二种聚合物HEC辅助组装,获得直径约500nm的片状聚集体。为了观察这种大片状聚集体的微结构形貌,我们提出在聚集体表面还原氯金酸并沉积金原子,增强衬度后再用TEM表征的方法。该法利用氯金酸能被具有弱还原性的大分子原位还原的特性,使金原子在聚集体表面及可能存在的多孔微结构处沉积,从而增强聚集体还原处的电镜表征衬度。金原位还原并沉积的TEM表征获得了清晰影像,证实上述pH响应性片状聚集体具有纳米多孔的微结构。采用同样方法还证明,在更低pH 0.9处,上述纳米多孔片状聚集体崩解为粒径约为10 nm的小胶体粒子。本实验证明金原位还原并沉积的TEM表征是一种观察低衬度或小粒度聚集体微结构形貌的有效方法。实验结果还证明,HPAM的“短亲水/疏水链段”的链分布特征,使其聚集体在水环境中具有短程且弥散性分布亲/疏水微区的特性,能够形成表面亲水微区较为富集、内部疏水微区较为富集,且内部还包含弥散性分布亲水微区的大复合聚集结构。以上述双亲性无规共聚物聚集体为微反应器合成金微纳结构,能够获得很有趣的金/聚合物复合微纳结构,具有空心或花状的特殊形貌。
Self-assembly of small-molecular surfactants into micelles with various morphologies and sizes has been one of the core subjects in colloid and interface science. However, in recent years complexation of surfactants and water-soluble homopolymers and their co-self-assembly has drawn much attention of the researchers in the field of colloid as well as polymer sciences. The interaction between homopolymers and surfactants changes the assembly performance of surfactants, and offers some new co-self-assembly architectures. In fact, these co-self-assemblies have been applied in life science, food and medicine, enhanced oil recovery, personal care products and nanomaterials, etc.
So far. studies on co-self-assemblies of water-soluble nonionic homopolymers and surfactants mainly focus on the discovery and verification of the dual-critical concentrations of surfactants, the sites of the interaction, and their miscellaneous applications. Nevertheless, it lacks of quantitative understanding of the processes of the complexation and co-self-asembly of the homopolymers and surfactant molecules. Therefore, one of the concerns in this dissertation is, can we investigate the co-self-assembly of surfactants and homopolymers leading to some quantitative results and clearly observe the microstructures and macrostructures of the co-self-assemblies?
It is reported that wet-chemical method is one of the main strategies to synthesize inorganic nanoparticles. Surfactants or water-soluble polymers have been used separately as capping agents in many wet-chemical methods while polymer/surfactant complexes have been tried as well. However, there still remains unclear in the functions of the polymer/surfactant complexes, which makes it difficult to control effectively the sizes and morphologies of the synthesized inorganic nanoparticles. Therefore, another concern in this dissertation is, could we use the homopolymer/surfactant complexes as microreactors to control the sizes and morphologies of the target metal micro/nano-particles based on our understanding of the microstructures and macrostructures of the polymer/surfactant co-self-assemblies?
Amphiphilic random copolymers demonstrate more potential in applications due to their low-cost and facile preparation. But much less attention has been paid to their self-assembly since their inherent feature of the "short hydrophilic/hydrophobic segment" makes it difficult to form clear core-shell structures as in block/graft copolymer micelles or noncovalently connected micelles. Thus, the third concern in this dissertation is, wether the simple amphiphilic random copolymers could assemble in aqueous solution into new aggregate architectures and if the assemblies have potential to apply as microreactors for metal micro/nano-particles?
Aiming at the aforementioned three concerns, this dissertation mainly focuses on the following:
1. The quantitative study on co-self-assembly between PVP or PEG and SDS
The aqueous solutions of PVP (polyvinylpyrrolidone)/SDS (sodium dodecyl sulfate) complex and PEG (polyethyleneglycol)/SDS complex were investigated with several methods including surface tension, electric conductivity, ultra filtration, solubilization and fluorescence molecular probe. Thus the characteristic parameters of the water-soluble nonionic homopolymer/SDS aggregates were obtained such as the first critical concentration of surfactant (c1), the second critical concentration of surfactant (C2) and N, the bound-micellar aggregation number of SDS. Three other novel characteristic parameters were inferred from the above experimental results, which describe the quantity ratios and the thresholds of the co-self-assemblies. That is. (1) Specific saturated bound capacity [B], the maximum number of homopolymer chain units bounded by each aggregated surfactant. (2) Critical bound-micellar aggregation number [N], the minimum bound-micellar aggregation number of SDS at c1.(3) Threshold molecular weight of polymer [M], the minimum polymer molecular weight required by co-self-assembly. The experimental results showed that the above three characteristic parameters are constants for given molecular structures of both surfactants and polymers, and independent of the molecular weights and concentrations of the homopolymers. The architecture of PVP/SDS co-self-assembly is deduced basically from NMR proofs, the critical concentrations, the above three characteristic parameters and some other supporting information got from cloud point, Krafft point and rheology data. Thus, PVP/SDS co-self-assembly was proposed to have a pseudo-polyelectrolyte microstructure and a necklace-like macro structure.
2. Application of PVP/SDS co-self-assemblies as microreactors
PVP/SDS co-self-assemblies could be used as microreactors for metal micro/nano-particles. It was found out that the pseudo-polyelectrolyte microstructure of the assemblies has the function to accumulate the precursor metal counterions, and its necklace-like macrostructure has the function to direct morphologies and sizes of the target metal micro/nano-particles. Various metal micro/nano-particles in quasi-3-D, 2-D,1-D as well as 0-D including gold, silver, nickel and copper were synthesized in PVP/SDS microreactor; and a synergistic morphology control strategy was developed depending on competition among crystal growth, direction by microreactor and infinitesimal disturbance by influence factors. These results make the homopolymer/surfactant microreactors effective and practical in regulating the target metal micro/nano-particles, and thus shade some light on the practicability of wet-chemical methods to synthesize metal micro/nano-particles.
3. pH responsive self-assembly of HPAM and their application as microreactors
pH responsive self-assembly of HPAM (partially hydrolyzed polyacrylamide) alone or assisted by HEC (hydroxyethylcellulose) in aqueous solution was investigated, which led to aggregate sheets in a size around 500 nm at pH 1.3. A new contrast enhancing strategy for clear TEM observation of the microstructure of the sheets was established and adopted. In this strategy, the added HAuCl4 was easy to be reduced by weakly reductive polymers in situ and then the resultant metal particles were doped on the external surface as well as the possible porous internal surface of the aggregate sheets leading to apparent increase of the contrast. The in situ reduction gold-doping TEM images announced that the pH responsive HPAM or HPAM/HEC aggregate sheets have nano-porous microstructures. Furthermore, the TEM observation disclosed that at a lower pH 0.9, the HPAM or HPAM/HEC aggregate sheets actually fall apart into nanoparticles about 10 nm. This in situ reduction gold-doping TEM observation strategy provides an efficient technique to directly detect low contrast microstructure or morphology of tiny organic assembly. In addition, the experiment results illustrated that the nature of "short hydrophilic/hydrophobic segment" in amphiphilic random copolymers induces short-range and dispersive hydrophilic/hydrophobic domains in the aggregates. In the resultant large complex aggregates, the hydrophobic and hydrophilic micro-domains enriched inside and on the surface of the aggregates, respectovely. Some interesting morphologies of the composites made of gold particles and the random copolymer such as hollow or flower-like ones, were obtained using the above amphiphilic random copolymer aggregates as microreactors.
研究表面活性剂与水溶性非离子均聚物的共同自组装,目前主要集中在对表面活性剂双临界浓度现象、两者间相互作用部位或其具体应用等方面,却少有对两者间自组装定量规律的研究。因此,本论文关注的第一个问题是：能否从定量层面考察均聚物与表面活性剂共同自组装行为,并探索共同自组装体的微结构和宏结构?
湿化学法是目前合成无机纳米材料的主要方法之一,其中大量使用表面活性剂或水溶性聚合物作包覆剂,目前也有一些同时使用两者作复合包覆剂的报导。但是,由于对复合包覆剂的功能不甚清楚,因而很难对目标无机纳米材料的尺度和形貌进行有效的调控。因此,本论文关注的第二个问题是：能否在深入了解水溶性非离子均聚物／表面活性剂共同自组装体微结构和宏结构的基础上,以其作为微反应器,调控其中目标金属还原产物的尺度和形貌?
双亲性无规共聚物廉价易得,较之于两亲嵌段共聚物或接枝共聚物而言更有潜在的应用价值。但双亲性无规共聚物具有“短亲/疏水链段”的链结构特点,使其不能形成类似于两亲嵌段共聚物或接枝共聚物胶束、或非共价键合胶束的明确核壳结构,因而在大分子自组装中少受关注。因此,本论文关注的第三个问题是：双亲性无规共聚物能否在完全水相环境中自组装成新的聚集构造以及用作制备金属微纳结构的微反应器的可能性?
围绕以上提出的三个问题,本论文的主要工作分为以下三个方面：
1、定量研究PVP或PEG与SDS的共同自组装
采用表面张力、电导率、超滤、增溶、荧光分子探针等研究手段,获得聚乙烯毗咯烷酮(PVP)/十二烷基硫酸钠(SDS)和聚乙二醇(PEG)/SDS复合体系水溶液中SDS的第一临界浓度c1、第二临界浓度c2和束缚胶束聚集数N等数据。研究水溶性非离子均聚物/表面活性剂的共同组装过程,得到三个主要特征参数,以其反映两者间共同自组装的边界和定量关系：(1)饱和束缚比[B],反映每个束缚胶束化SDS分子结合均聚物链节的最大能力；(2)临界束缚胶束聚集数[N],反映均聚物上形成SDS束缚胶束的最小聚集数；(3)聚合物分子量阈值[M],反映共同自组装所要求的最小聚合物分子量。实验事实表明,上述三个新特征参数都是只由表面活性剂及均聚物的分子结构确定的不变量,而受聚合物分子量([M]除外)和浓度等的影响很小。综合SDS的临界浓度、三个特征参数与核磁共振、浊点、克拉夫特点以及流变性等实验结果,证明PVP/SDS共同自组装体既具有“拟聚电解质”微结构,又具有项链状宏结构。
2、PVP/SDS共同自组装体的微反应器应用
将PVP/SDS共同自组装体作为制备金属微纳结构的微反应器,发现该微反应器的“拟聚电解质”微结构具有富集金属反离子功能,其项链状宏结构可以发挥调控金属还原产物的形貌和尺度的功能。在PVP/SDS微反应器中,借助晶体生长、微反应器调控与环境影响因素等因子之间的竞争和协同作用,合成了金、银、镍、铜等元素的准3-D、2-D、1-D乃至0-D金属微纳结构,从而在同一种微反应器中分别获得了多种成分、多种维度以及多种形貌的金属微纳结构。本研究结果表明,使用水溶性非离子均聚物/表面活性剂自组装体作微反应器,可对生成的金属微纳结构实施更有效的调控,这对推进湿化学方法制备金属微纳结构具有较大实用意义。
3、HPAM的pH响应性自组装及微反应器应用
考察部分水解聚丙烯酰胺(HPAM)在水相中的pH响应性自组装行为。在pH诱导下,HPAM在水相中能够独自组装、或经第二种聚合物HEC辅助组装,获得直径约500nm的片状聚集体。为了观察这种大片状聚集体的微结构形貌,我们提出在聚集体表面还原氯金酸并沉积金原子,增强衬度后再用TEM表征的方法。该法利用氯金酸能被具有弱还原性的大分子原位还原的特性,使金原子在聚集体表面及可能存在的多孔微结构处沉积,从而增强聚集体还原处的电镜表征衬度。金原位还原并沉积的TEM表征获得了清晰影像,证实上述pH响应性片状聚集体具有纳米多孔的微结构。采用同样方法还证明,在更低pH 0.9处,上述纳米多孔片状聚集体崩解为粒径约为10 nm的小胶体粒子。本实验证明金原位还原并沉积的TEM表征是一种观察低衬度或小粒度聚集体微结构形貌的有效方法。实验结果还证明,HPAM的“短亲水/疏水链段”的链分布特征,使其聚集体在水环境中具有短程且弥散性分布亲/疏水微区的特性,能够形成表面亲水微区较为富集、内部疏水微区较为富集,且内部还包含弥散性分布亲水微区的大复合聚集结构。以上述双亲性无规共聚物聚集体为微反应器合成金微纳结构,能够获得很有趣的金/聚合物复合微纳结构,具有空心或花状的特殊形貌。
Self-assembly of small-molecular surfactants into micelles with various morphologies and sizes has been one of the core subjects in colloid and interface science. However, in recent years complexation of surfactants and water-soluble homopolymers and their co-self-assembly has drawn much attention of the researchers in the field of colloid as well as polymer sciences. The interaction between homopolymers and surfactants changes the assembly performance of surfactants, and offers some new co-self-assembly architectures. In fact, these co-self-assemblies have been applied in life science, food and medicine, enhanced oil recovery, personal care products and nanomaterials, etc.
So far. studies on co-self-assemblies of water-soluble nonionic homopolymers and surfactants mainly focus on the discovery and verification of the dual-critical concentrations of surfactants, the sites of the interaction, and their miscellaneous applications. Nevertheless, it lacks of quantitative understanding of the processes of the complexation and co-self-asembly of the homopolymers and surfactant molecules. Therefore, one of the concerns in this dissertation is, can we investigate the co-self-assembly of surfactants and homopolymers leading to some quantitative results and clearly observe the microstructures and macrostructures of the co-self-assemblies?
It is reported that wet-chemical method is one of the main strategies to synthesize inorganic nanoparticles. Surfactants or water-soluble polymers have been used separately as capping agents in many wet-chemical methods while polymer/surfactant complexes have been tried as well. However, there still remains unclear in the functions of the polymer/surfactant complexes, which makes it difficult to control effectively the sizes and morphologies of the synthesized inorganic nanoparticles. Therefore, another concern in this dissertation is, could we use the homopolymer/surfactant complexes as microreactors to control the sizes and morphologies of the target metal micro/nano-particles based on our understanding of the microstructures and macrostructures of the polymer/surfactant co-self-assemblies?
Amphiphilic random copolymers demonstrate more potential in applications due to their low-cost and facile preparation. But much less attention has been paid to their self-assembly since their inherent feature of the "short hydrophilic/hydrophobic segment" makes it difficult to form clear core-shell structures as in block/graft copolymer micelles or noncovalently connected micelles. Thus, the third concern in this dissertation is, wether the simple amphiphilic random copolymers could assemble in aqueous solution into new aggregate architectures and if the assemblies have potential to apply as microreactors for metal micro/nano-particles?
Aiming at the aforementioned three concerns, this dissertation mainly focuses on the following:
1. The quantitative study on co-self-assembly between PVP or PEG and SDS
The aqueous solutions of PVP (polyvinylpyrrolidone)/SDS (sodium dodecyl sulfate) complex and PEG (polyethyleneglycol)/SDS complex were investigated with several methods including surface tension, electric conductivity, ultra filtration, solubilization and fluorescence molecular probe. Thus the characteristic parameters of the water-soluble nonionic homopolymer/SDS aggregates were obtained such as the first critical concentration of surfactant (c1), the second critical concentration of surfactant (C2) and N, the bound-micellar aggregation number of SDS. Three other novel characteristic parameters were inferred from the above experimental results, which describe the quantity ratios and the thresholds of the co-self-assemblies. That is. (1) Specific saturated bound capacity [B], the maximum number of homopolymer chain units bounded by each aggregated surfactant. (2) Critical bound-micellar aggregation number [N], the minimum bound-micellar aggregation number of SDS at c1.(3) Threshold molecular weight of polymer [M], the minimum polymer molecular weight required by co-self-assembly. The experimental results showed that the above three characteristic parameters are constants for given molecular structures of both surfactants and polymers, and independent of the molecular weights and concentrations of the homopolymers. The architecture of PVP/SDS co-self-assembly is deduced basically from NMR proofs, the critical concentrations, the above three characteristic parameters and some other supporting information got from cloud point, Krafft point and rheology data. Thus, PVP/SDS co-self-assembly was proposed to have a pseudo-polyelectrolyte microstructure and a necklace-like macro structure.
2. Application of PVP/SDS co-self-assemblies as microreactors
PVP/SDS co-self-assemblies could be used as microreactors for metal micro/nano-particles. It was found out that the pseudo-polyelectrolyte microstructure of the assemblies has the function to accumulate the precursor metal counterions, and its necklace-like macrostructure has the function to direct morphologies and sizes of the target metal micro/nano-particles. Various metal micro/nano-particles in quasi-3-D, 2-D,1-D as well as 0-D including gold, silver, nickel and copper were synthesized in PVP/SDS microreactor; and a synergistic morphology control strategy was developed depending on competition among crystal growth, direction by microreactor and infinitesimal disturbance by influence factors. These results make the homopolymer/surfactant microreactors effective and practical in regulating the target metal micro/nano-particles, and thus shade some light on the practicability of wet-chemical methods to synthesize metal micro/nano-particles.
3. pH responsive self-assembly of HPAM and their application as microreactors
pH responsive self-assembly of HPAM (partially hydrolyzed polyacrylamide) alone or assisted by HEC (hydroxyethylcellulose) in aqueous solution was investigated, which led to aggregate sheets in a size around 500 nm at pH 1.3. A new contrast enhancing strategy for clear TEM observation of the microstructure of the sheets was established and adopted. In this strategy, the added HAuCl4 was easy to be reduced by weakly reductive polymers in situ and then the resultant metal particles were doped on the external surface as well as the possible porous internal surface of the aggregate sheets leading to apparent increase of the contrast. The in situ reduction gold-doping TEM images announced that the pH responsive HPAM or HPAM/HEC aggregate sheets have nano-porous microstructures. Furthermore, the TEM observation disclosed that at a lower pH 0.9, the HPAM or HPAM/HEC aggregate sheets actually fall apart into nanoparticles about 10 nm. This in situ reduction gold-doping TEM observation strategy provides an efficient technique to directly detect low contrast microstructure or morphology of tiny organic assembly. In addition, the experiment results illustrated that the nature of "short hydrophilic/hydrophobic segment" in amphiphilic random copolymers induces short-range and dispersive hydrophilic/hydrophobic domains in the aggregates. In the resultant large complex aggregates, the hydrophobic and hydrophilic micro-domains enriched inside and on the surface of the aggregates, respectovely. Some interesting morphologies of the composites made of gold particles and the random copolymer such as hollow or flower-like ones, were obtained using the above amphiphilic random copolymer aggregates as microreactors.
引文
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